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MARS 6 Microwave Acid Digestion Method Note Compendium October 1, 2019

Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

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Page 1: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

MARS 6Microwave Acid Digestion

Method Note Compendium

October 1, 2019

Page 2: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Contents

Agriculture

Alfalfa 11

Boric Acid HF Neutralization 12

Cannabis (Plant) 13

Coffee Beans 14

Cotton 15

Feed Grain 16

Fertilizer - AOAC Method 2017.02 17

Fertilizer -AOAC Method 2006.03 18

Geranium 19

Impatiens 20

Leather 21

Palm Leaves 22

Plant Tissue 23

Soybean 24

Soybean Meal 25

Spinach Leaves 26

Straw 27

Tea Extract 28

Tea Tannin 29

Tobacco 30

Wheat 31

Wood 32

Wood Pulp 33

Wool 34

Yeast 35

Clinical & Biological

Animal Tissue (Dry) 37

Animal Tissue (Wet) 38

Beef Bone 39

Blood (Human) 40

Bovine Blood 42

Bovine Liver (Wet) 43

Brain Tissue (Dog) 44

Dog Feces (Dry) 45

Fingernails 46

Hair 47

Lobster Hepatopancreas (Tort-CRM) 48

Rat Kidney 49

Urine - Human 50

Consumer Products

Boric Acid HF Neutralization 52

Candle Fragrance in iPrep 53

Cosmetics (Liquid Make-Up) 54

Cotton 55

Deodorant (Powder) 56

Eye Shadow 57

Foam (Mattress) in iPrep 58

Sanitizers (Hand) 59

Shampoo (Dandruff) 60

Soaps (Lotion and Foam) 61

Sunscreen in iPrep 62

Suppository (Capsule) 63

Toothpaste 64

Vaseline 65

Wax (Candle) 66

Environmental & Regulatory

Boric Acid HF Neutralization 68

Fertilizer - AOAC Method 2017.02 69

Fertilizer - AOAC Method 2006.03 70

Fly Ash in iPrep 71

Limestone 73

Page 3: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

NPDES (Waste Water) 74

Pine Needles 75

RoHS (For Pb, Hg, and Cd Analysis) 76

Sediment (BCCS - 1 CRM) (Leach) 77

Sediment (Buffalo River) (Leach) 78

Sludge (Industrial) 79

Soil (Montana - CRM) (Leach) 80

TCLP Extract 81

US EPA 3015 (Aqueous Samples) 82

US EPA 3015a (Aqueous Sample) 83

US EPA 3051 (Solid Sample) 84

US EPA 3051a (Solid Sample) 85

US EPA 3052 (Sludge, Soil, Sediment or Oil) 86

USP 232/233 (Pharmaceuticals) 87

Waste Activated Sludge 88

Water (For Analysis of Phosphorous) 89

Wood 90

Food Testing

Alum 92

Apple 93

Asparagus 94

Aspartame in iPrep 95

Bacon (Cooked) 96

Beef (Ground) 97

Beef Bouillon 98

Beer (Light) 99

Blueberry 100

Broccoli 101

Caramel Color 102

Carrot 103

Celery 104

Cheese (Cracker) 105

Cheese (Powder) 106

Cheese (Processed) 107

Cherry 108

Chewing Gum 109

Chicken (Boneless) 110

Chili Candy (Mexican) 111

Chili Powder in iPrep 112

Chips (Potato) 113

Citrus Leaves 114

Clam Puree 115

Cocoa 116

Coconut 117

Coffee Beans 118

Cucumber 119

Dog Food 120

Fish Tissue 121

Flounder 122

Flour 123

Food 124

Food Coloring (Liquid) 125

Fruit Juice 126

Gelatin 127

Granola Bar 128

Grape 129

Grapefruit 130

Gummy Bear 131

Ham 132

Infant Cereal (Rice Grain) 133

Infant Formula (Liquid) in iPrep 134

Infant Formula (Liquid) 135

Infant Formula (Powder) in iPrep 136

Infant Formula (Powder) 137

Kidney Bean 138

Kielbasa Sausage 139

Maple Syrup 140

Mayonnaise 141

Meal Replacement Shake (Chocolate) 142

Milk (Whole - Liquid) 143

Page 4: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Milk (Powder) 144

Nutritional Drink (Adult) 145

Olive Oil 146

Orange Juice 147

Oyster Puree 148

Peanut Butter 149

Pear 150

Pepper (Bell, Chili, Etc.) 151

Pistachio Nuts 152

Pizza (Frozen, Pepperoni) 153

Plum 154

Pork (Ground) 155

Potato 156

Potato Chips 157

Pretzel (Salted) 158

Protein Bar 159

Raspberry 160

Rice 161

Safflower Oil 162

Salad Dressing (Ranch) 163

Salami 164

Sausage 165

Soda (Diet) 166

Sodium Free - Seasoning 167

Soybean 168

Spinach 169

Spinach Leaves 170

Spinach Pasta 171

Strawberry 172

Sugar (Granulated) 173

Tea (Chai) in iPrep 174

Tea Leaves 175

Tomato Leaves 176

Tomato Paste (70% Moisture) 177

Tomato Soup 178

Walnut 179

Watermelon 180

Wheat Crackers 181

Whey 182

Whey (Powder) 183

Wine 184

Yogurt (Plain) 185

Geoscience & Mining

Alpha - Alumina in iPrep 187

Alumina Beads (with Silver Substrate) in iPrep 188

Alumina Powder in iPrep 190

Aluminum Nitride 191

Aluminum Oxide 192

Aluminum Oxide (H3PO4) in iPrep 193

Asbestos 194

Automotive Catalyst 195

Barium Titanate (BaTiO3) 196

Bastnaesite Ore 197

Bauxite 199

Bismuth Aluminate Mixture 201

Bismuth Yttrium Iron Oxide in iPrep 202

Boiler Scale (80-90% Fe) 204

Boric Acid HF Neutralization 205

Boron Carbide (B4C) in iPrep 206

Carbon 207

Cement 208

Ceramic (Fused Silica) 209

Ceramics 210

Char - Sulfuric Acid 211

Chromium Carbide 212

Chromium Oxide (Cr2O3) in iPrep 213

Clay 214

Coal in iPrep 215

Coal 216

Coal Ash 217

Page 5: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Cryolite / Electrolytic Bath 218

Feldspar in iPrep 220

Ferric Oxide in iPrep 222

Furnace Slag 223

Gadolinium Zirconium Oxide in iPrep 224

Gas Atomized Powder in iPrep 226

Glass Fiber 227

Hafnium Oxide 228

Ilmenite (FeTiO3) 229

Iron Ore 230

Kaolin 231

Kerosene 232

Lead Sulfide (PbS) 233

Lithium Nickel Cobalt Manganese Oxide 234

Magnesium Oxide (MgO 40-54%) 235

Manganous Oxide (MnO) 236

Mica in iPrep 238

Mill Tailings 239

Mineral Ore 241

Molybdenum Disulfide (MoS2) 243

Nickel (II) Hydroxide 245

Niobium Pentoxide 246

Petroleum Coke 247

Phosphate (21%) 249

Phosphate Rock 250

Pollucite Ore in iPrep 251

Pyrophyllite (AlSi2)5(OH) 253

Quartz Powder 254

Rock (Pulverized) 255

Rock, High Sulfide in iPrep 256

Rutile Ore 258

Sand 259

Shale in iPrep 260

Silica Sand 261

Silica Sand in iPrep 262

Silicon Dioxide 263

Silicon Nitride in iPrep 264

Silicon Wafer 265

Slag - Furnace 266

Sodium Antimonate in iPrep 267

Spodumene (Lithium Feldspar) 268

Sulfide Bulk Concentrate in iPrep 270

Tantalum Pentoxide (Ta2O5) in iPrep 272

Titanium Dioxide 273

Titanium Slag Ore in iPrep 274

Tungsten Carbide 275

Tungsten Ore (50% W; 10% Fe; 2% Mn) 276

Tungsten Oxide 277

Vermiculite 278

Wollastonite (Calcium Silicate) in iPrep 279

Zeolite 280

Zinc Oxide (ZnO) 281

Zinc Oxide (ZnO) in iPrep 282

Zircon in iPrep 283

Industrial Hygiene

Asbestos 285

Filter (MCE) 286

Filter Paper - 37 mm Mixed Cellulose Ester 287

Filter Paper - 47 mm Polycarbonate 288

Filter Paper - Cellulose 289

Ghost Wipe 290

Paint Chips (For Pb Analysis) 291

Quartz Fiber Filters 292

Toray Filter in iPrep 293

Toray Filter (Anion) 294

Toray Filter (Cation) 295

Materials Science

Acrylic Tape in iPrep 297

Page 6: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Bismuth Aluminate Mixture 298

Bismuth Yttrium Iron Oxide in iPrep 299

Ceramic Powder 301

Ceramic Powder in iPrep 302

Circuit Board (Cryo - Ground) 303

Ferric Oxide in iPrep 304

Gadolinium Zirconium Oxide in iPrep 305

Gas Atomized Powder in iPrep 307

Glass (Ground) 308

Graphite Composite - Cyanate Ester Resin 309

Graphite Composite - Epoxy Resin 310

Graphite Composite - PEEK Resin 311

Graphite Fiber - Cyanate Siloxane Resin 312

Graphite Fiber - Epoxy Resin (Fiber Content) 313

Pollucite Ore in iPrep 314

Siloxanes 316

Metals & Alloys

Alpha - Alumina in iPrep 318

Aluminum (Metal) 319

Aluminum Alloy 320

Aluminum Alloy (20% SiC) 321

Aluminum Alloy (BCS 182) 322

Aluminum Oxide 323

Aluminum Oxide (H3PO4) in iPrep 324

Boron 325

Boron Carbide (B4C) in iPrep 326

Carbonyl Iron in iPrep 327

Cobalt - Chromium Alloy (Co-Cr) 328

Copper (Metal) 330

Copper Ore 331

Gallium 332

Iron - Chromium Alloy 333

Iron - Chromium Alloy in iPrep 335

Iron - Lignosulfonate 336

Iron - Manganese Alloy 337

Iron - Silicon Alloy 338

Lead Sulfide (PbS) 339

Lithium Nickel Cobalt Manganese Oxide 340

Magnesium Oxide (MgO 40-54%) 341

Manganous Oxide (MnO) 342

Metal Alloy - FeCr 344

Metal Alloy - NiCr 345

Metal Alloy (Ag, Au, Cu) in iPrep 346

Metal Alloy (Ag, Co, Cu) in iPrep 347

Metal Alloy (Ag, Cu, Sn) in iPrep 348

Metal Ore - Precious 349

Metals Alloy (Co-Cr) 351

Nickel (II) Hydroxide 353

Nickel (Metal) 354

Niobium - Titanium Alloy 355

Phosphate (21%) 356

Platinum Metal 357

Platinum Ruthenium in iPrep 358

Rhodium Sponge in iPrep 359

Selenium Alloy 360

Sn - Ag Solder 361

Stainless and Low Carbon Steel in iPrep 362

Stainless Steel 363

Steel (Stainless) 364

Strontium Ferrite in iPrep 365

Titanium Alloy 366

Titanium Dioxide 367

Tungsten Ore (50% W; 10% Fe; 2% Mn) 368

Zinc Oxide (ZnO) 369

Zinc Oxide (ZnO) in iPrep 370

Zircon Alloy 371

Nutraceuticals

Biotin 373

Page 7: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Cannabis (Plant) 374

Chili Powder in iPrep 375

Citrus Leaves 376

Ginkgo (Ground) 377

Ginkgo (Whole Pill) 378

Infant Formula (Liquid) in iPrep 379

Infant Formula (Liquid) 380

Infant Formula (Powder) in iPrep 381

Infant Formula (Powder) 382

Kelp 383

Milk (Whole - Liquid) 384

Milk (Powder) 385

Plant Tissue 386

USP 232/233 (Pharmaceuticals) 387

Wheat 388

Whey (Powder) 389

Organic Chemicals

Di-(2-ethylhexyl)phosphoric Acid in iPrep 391

Diazo Sulfonyl Chloride 392

Food Coloring (Erythrosine Based) 393

Methylcellulose (Hydroxypropyl) 394

Monoethanolamine 395

Photoresist 396

Polygluteramide 397

Paints & Coatings

Paint (Latex Based Liquid) 399

Paint Chips (For Pb Analysis) 400

Photoresist 401

Polyurethane 402

Polyurethane in iPrep 403

Toner (Ink) in iPrep 404

Toner (Powder) in iPrep 405

Paper & Pulp

Filter Paper - 37 mm Mixed Cellulose Ester 407

Filter Paper - 47 mm Polycarbonate 408

Filter Paper - Cellulose 409

Paper Pulp 410

Personal Care

Boric Acid HF Neutralization 412

Cosmetics (Liquid Make-Up) 413

Eye Shadow 414

Shampoo (Dandruff) 415

Pharmaceutical & Biotech

Allergy Pill (Ground) 417

Allergy Pill (Whole Pill) 418

Antioxidant (Ground) 419

Antioxidant (Whole Pill) 420

APIs with Aromatic Ring Structures in iPrep 421

Ascorbic Acid 422

Aspirin (Ground) 423

Aspirin (Whole) 424

Beta Carotene 425

Biotin 426

Calcium Carbonate 427

Calpan Pantothenic Acid 428

Cephalexin 429

Chromium Chelate 430

Cold & Flu Medicine (Liquid) 431

Cupric Sulfate 432

Diclofenac K 433

Empty Capsule (Gel) 434

Page 8: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Erythromycin 435

Fish Oil (No Capsule) 436

Flurbiprofen 437

Folic Acid 438

Ginkgo (Ground) 439

Ginkgo (Whole Pill) 440

Hydrocodone 441

Ibuprofen (Ground) 442

Kelp 443

Losartan K 444

Magnesium Carbonate 445

Magnesium Oxide 446

Manganese Carbonate 447

Medroxyprogesterone 448

Metformin (Ground) 449

Mineral Oil 450

Multivitamin (Ground) 451

Multivitamin (Whole) 452

Naproxen Sodium 453

Niacinamide 454

Pantothenic Acid 455

Potassium Chelate 456

Protopic Ointment 457

Pyridoxine 458

Riboflavin 459

Selenium Chelate 460

Sleep Aid 461

Sodium Polystyrene Sulfonate in iPrep 462

Stearic Acid 463

Sudan Orange (4-Fluorophenyl) in iPrep 464

Thiamine 465

Transdermal Patch 466

Trixie Phosphate in iPrep 467

USP 232/233 (Pharmaceuticals) 468

Vitamin B-12 469

Vitamin C (Ground) 470

Vitamin C (Whole) 471

Vitamin Concentrate (High Fe) 472

Vitamin D 473

Vitamin D3 474

Vitamin E 475

Vitamins 476

Zinc Sulfate 477

Plastics, Polymers, & Oils

Acrylamide 479

Brominated Flame Retardant in iPrep 480

Bunker Oil in iPrep 481

Char - Sulfuric Acid 482

Crude Oil 483

Diesel Fuel 484

Epoxy Hardener 485

Fatty Alcohol 486

Fluorinated Ethylene Propylene (FEP) in iPrep 487

Fuel Oil (Slurry) in iPrep 488

Gasoline 490

Glycerol Ester of Wood Rosin (Ground) in iPrep 491

HDPE 492

Kerosene 493

Kevlar in iPrep 494

Lube Oil 495

Methyl Ester of Hydrogenated Wood Rosin (Ground) in iPrep 496

Mineral Oil 497

Motor Oil (New) 498

Motor Oil (Waste) 499

Motor Oil (Waste) in iPrep 500

Nylon 501

Oil Wear Metals 502

PET (Polyethylene Terephthalate) 503

Page 9: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

PET (Polyethylene Terephthalate) in iPrep 504

Petrolatum 505

Plasticizer (Filter) in iPrep 506

Plasticizers in iPrep 507

Polycarbonate Resin 508

Polyethersulfone (Filter Paper) 510

Polyethylene - High Density 511

Polyphenylene Sulfide 512

Polypropylene 513

Polyterpene Resin in iPrep 514

Polyurethane 515

Polyurethane in iPrep 516

PVC (Polyvinyl Chloride Resin) 517

Rubber 518

Rubber (Synthetic) 519

Silane Terminated Polyether in iPrep 520

Silicone Tubing - TiO2 Filler 521

Styrene Acrylate 522

Terephthalic Acid 523

Wax (Petroleum Based) 524

Water & Wastewater Treatment

NPDES (Waste Water) 526

Sludge (Industrial) 527

TCLP Extract 528

US EPA 3015 (Aqueous Samples) 529

US EPA 3015a (Aqueous Sample) 530

Waste Activated Sludge 531

Water (For Analysis of Phosphorous) 532

Page 10: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Agriculture

Page 11: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

11

Microwave Digestion ofAlfalfa

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

520

Microwave Digestion ofAlfalfa

Page 12: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

12

Microwave Digestion ofBoric Acid HF Neutralization

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample WeightVaries by Sample

ReagentsH₃BO₃ (4%)

Recommended VesselsEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction of certain analytes with hydrofluoric acid.

Alternatively, 1-4 g of solid H₃BO₃ + 25 mL deionized H₂O can be used in place of the 4% w/v solution.

ProcedureAllow vessel to cool. Add 30 mL H₃BO₃ (4%) into the vessel that contains the sample and acid.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSee sample specific method notes.

6

Microwave Digestion ofBoric Acid HF Neutralization

Page 13: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

13

Microwave Digestion ofCannabis (Plant)

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃, or alternatively 9 mL HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

715

Microwave Digestion ofCannabis (Plant)

Page 14: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

14

Microwave Digestion ofCoffee Beans

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may; however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of ground sample into the digestion vessel. Add 10 ml of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 ml.

10

Microwave Digestion ofCoffee Beans

Page 15: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

15

Microwave Digestion ofCotton

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

231

Microwave Digestion ofCotton

Page 16: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

16

Microwave Digestion ofFeed Grain

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 ml of HNO₃, and 2 ml of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

232

Microwave Digestion ofFeed Grain

Page 17: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

17

Microwave Digestion ofFertilizer - AOAC Method 2017.02

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis. This method may not provide a total digest of all fertilizer samples.

ProcedureWeigh 1 g (0.5 g for organic matrices) of the sample into the digestion vessel. Add 9 mL of HNO₃, and 3 mL HCl. Gently swirl the mixture and wait approximately 20 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, with some particles (silicates) remaining upon dilution to 50 mL.

535

Microwave Digestion ofFertilizer - AOAC Method 2017.02

Page 18: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

18

Microwave Digestion ofFertilizer -AOAC Method 2006.03

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis method may not provide a total digest of all fertilizer samples.

ProcedureWeigh 1 g (0.5 g for organic matrices) of the sample into the digestion vessel. Add 10 ml of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

233

Microwave Digestion ofFertilizer -AOAC Method 2006.03

Page 19: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

19

Microwave Digestion ofGeranium

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900 -1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

521

Microwave Digestion ofGeranium

Page 20: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

20

Microwave Digestion ofImpatiens

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

522

Microwave Digestion ofImpatiens

Page 21: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

21

Microwave Digestion ofLeather

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

490

Microwave Digestion ofLeather

Page 22: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

22

Microwave Digestion ofPalm Leaves

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL HNO₃, and 2 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

523

Microwave Digestion ofPalm Leaves

Page 23: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

23

Microwave Digestion ofPlant Tissue

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis. Some plant tissues contain silicates which would require HF for total dissolution.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

234

Microwave Digestion ofPlant Tissue

Page 24: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

24

Microwave Digestion ofSoybean

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of (dry weight) sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

235

Microwave Digestion ofSoybean

Page 25: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

25

Microwave Digestion ofSoybean Meal

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

524

Microwave Digestion ofSoybean Meal

Page 26: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

26

Microwave Digestion ofSpinach Leaves

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis. Some plant tissues contain silicates which would require HF for total dissolution.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 ml of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 ml.

236

Microwave Digestion ofSpinach Leaves

Page 27: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

27

Microwave Digestion ofStraw

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization” The addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 ml of HNO₃, and 1 ml of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 ml.

237

Microwave Digestion ofStraw

Page 28: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

28

Microwave Digestion ofTea Extract

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

525

Microwave Digestion ofTea Extract

Page 29: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

29

Microwave Digestion ofTea Tannin

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL HNO₃ and 1 mL HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

526

Microwave Digestion ofTea Tannin

Page 30: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

30

Microwave Digestion ofTobacco

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

238

Microwave Digestion ofTobacco

Page 31: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

31

Microwave Digestion ofWheat

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

239

Microwave Digestion ofWheat

Page 32: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

32

Microwave Digestion ofWood

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

268

Microwave Digestion ofWood

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33

Microwave Digestion ofWood Pulp

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Wet Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (wet weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

527

Microwave Digestion ofWood Pulp

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34

Microwave Digestion ofWool

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

528

Microwave Digestion ofWool

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35

Microwave Digestion ofYeast

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1.0 g of dry weight (0.5 g w/Xpress vessels) into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

240

Microwave Digestion ofYeast

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Clinical & Biological

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Microwave Digestion ofAnimal Tissue (Dry)

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may; however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g (0.25 g w/MARSXpress Vessels) into the digestion vessel. Add 10 ml of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 ml.

4

37

Microwave Digestion ofAnimal Tissue (Dry)

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Microwave Digestion ofAnimal Tissue (Wet)

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 g (0.5 g w Xpress Vessels) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

241

38

Microwave Digestion ofAnimal Tissue (Wet)

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Microwave Digestion ofBeef Bone

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Ground)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (ground) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

529

39

Microwave Digestion ofBeef Bone

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Microwave Digestion ofBlood (Human)

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2 mL

ReagentsHNO₃ H₂O₂

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesTake caution when mixing the acids and the sample. The sample may foam slightly.

ProcedureTransfer 2 mL of the sample into the digestion vessel. Add 5 mL of HNO₃ and 2 mL of H₂O₂. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

242

40

Microwave Digestion ofBlood (Human)

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Microwave Digestion ofBlood (Human)

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 mL

ReagentsHNO₃

Recommended Vessels10 mL MARSXpress20 mL MARSXpress

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 0.5 mL of the sample into the digestion vessel. Add 2 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 N/A 1030-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.c) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

737

41

Microwave Digestion ofBlood (Human)

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Microwave Digestion ofBovine Blood

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 1 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

531

42

Microwave Digestion ofBovine Blood

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Microwave Digestion ofBovine Liver (Wet)

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g (Wet Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1.0 g (wet weight )(0.5 g w/Xpress Vessels) into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

243

43

Microwave Digestion ofBovine Liver (Wet)

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Microwave Digestion ofBrain Tissue (Dog)

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g (Wet Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1 g (wet weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

532

44

Microwave Digestion ofBrain Tissue (Dog)

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Microwave Digestion ofDog Feces (Dry)

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.2 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

533

45

Microwave Digestion ofDog Feces (Dry)

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Microwave Digestion ofFingernails

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃

Recommended Vessels10 mL MARSXpress20 mL MARSXpress

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.1 g (0.05 g if using the 10 mL vessel) of the sample into the digestion vessel. Add 4 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 15:00 N/A 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.c) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

741

46

Microwave Digestion ofFingernails

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Microwave Digestion ofHair

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃

Recommended Vessels10 mL MARSXpress20 mL MARSXpress

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.1 g (0.05 g if using the 10 mL vessel) of the sample into the digestion vessel. Add 4 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 15:00 N/A 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.c) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

740

47

Microwave Digestion ofHair

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Microwave Digestion ofLobster Hepatopancreas (Tort-CRM)

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1.0 g (dry weight) (0.5 g w/Xpress Vessels) into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

244

48

Microwave Digestion ofLobster Hepatopancreas (Tort-CRM)

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Microwave Digestion ofRat Kidney

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g (Wet Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1 g (wet weight) of the sample into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

534

49

Microwave Digestion ofRat Kidney

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Microwave Digestion ofUrine - Human

Clinical aMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight4 mL

ReagentsHNO₃H₂O₂

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesTake caution when mixing the acids and the sample. The sample may foam slightly.

ProcedureTransfer 4 ml of the sample into the digestion vessel. Add 4 mL of HNO₃, and 2 mL of H₂O₂. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 ml.

245

50

Microwave Digestion ofUrine - Human

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Consumer Products

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52

Microwave Digestion ofBoric Acid HF Neutralization

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample WeightVaries by Sample

ReagentsH₃BO₃ (4%)

Recommended VesselsEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction of certain analytes with hydrofluoric acid.

Alternatively, 1-4 g of solid H₃BO₃ + 25 mL deionized H₂O can be used in place of the 4% w/v solution.

ProcedureAllow vessel to cool. Add 30 mL H₃BO₃ (4%) into the vessel that contains the sample and acid.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSee sample specific method notes.

6

Microwave Digestion ofBoric Acid HF Neutralization

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53

Microwave Digestion ofCandle Fragrance

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution.The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureAdd 0.1 g of the sample into the digestion vessel. Add 7 mL of HNO₃ and 1 mL HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 250 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and colorless upon dilution to 50 mL.

676

Microwave Digestion ofCandle Fragrance in iPrep

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54

Microwave Digestion ofCosmetics (Liquid Make-Up)

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 8 mL of HNO₃ and 2 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

246

Microwave Digestion ofCosmetics (Liquid Make-Up)

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55

Microwave Digestion ofCotton

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

231

Microwave Digestion ofCotton

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56

Microwave Digestion ofDeodorant (Powder)

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 2 mL of HNO₃ and 6 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 25:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

735

Microwave Digestion ofDeodorant (Powder)

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57

Microwave Digestion ofEye Shadow

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 7 mL of HNO₃ and 3 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL

247

Microwave Digestion ofEye Shadow

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58

Microwave Digestion ofFoam (Mattress)

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃H₂SO₄

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL HNO₃ and 1 mL of H₂SO₄. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 250 30:00 15:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

670

Microwave Digestion ofFoam (Mattress) in iPrep

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59

Microwave Digestion ofSanitizers (Hand)

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHClHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesAcid addition should be added slowly and in aliquots of 1 mL, as the reaction is vigorous and exothermic upon addition of HNO₃.The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution.The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 1 mL of HCl and 4 mL of HNO₃ in aliquots of 1 mL. Gently swirl after each aliquot is added and allow reaction to subside before adding more HNO3. Allow approximately 45 minutes for pre-digestion.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 190 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

755

Microwave Digestion ofSanitizers (Hand)

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60

Microwave Digestion ofShampoo (Dandruff)

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe use of HF may be required to digest any silicates found in the sample.

ProcedureTransfer 1 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

248

Microwave Digestion ofShampoo (Dandruff)

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61

Microwave Digestion ofSoaps (Lotion and Foam)

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 4 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 190 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

754

Microwave Digestion ofSoaps (Lotion and Foam)

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62

Microwave Digestion ofSunscreen

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 8 mL of HNO₃ and 2 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 30:00 15:00 N/A 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 250 mL.

756

Microwave Digestion ofSunscreen in iPrep

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63

Microwave Digestion ofSuppository (Capsule)

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Capsule (Approx 1 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesEnsure that the capsule is completely covered with reagent before sealing the vessel.

ProcedureWeigh 1 Capsule (approx. 1.0 g) into the digestion vessel. Add 12 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

249

Microwave Digestion ofSuppository (Capsule)

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64

Microwave Digestion ofToothpaste

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.1 g of the sample onto a filter disk and insert into the digestion vessel. Add 8 mL HNO₃ and 2 mL HF. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 15:00 800 1030-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) The control / reference vessel must contain the largest and most reactive sample.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

733

Microwave Digestion ofToothpaste

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65

Microwave Digestion ofVaseline

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

250

Microwave Digestion ofVaseline

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66

Microwave Digestion ofWax (Candle)

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

251

Microwave Digestion ofWax (Candle)

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Environmental & Regulatory

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Microwave Digestion ofBoric Acid HF Neutralization

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample WeightVaries by Sample

ReagentsH₃BO₃ (4%)

Recommended VesselsEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction of certain analytes with hydrofluoric acid.

Alternatively, 1-4 g of solid H₃BO₃ + 25 mL deionized H₂O can be used in place of the 4% w/v solution.

ProcedureAllow vessel to cool. Add 30 mL H₃BO₃ (4%) into the vessel that contains the sample and acid.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSee sample specific method notes.

6

68

Microwave Digestion ofBoric Acid HF Neutralization

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Microwave Digestion ofFertilizer - AOAC Method 2017.02

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis. This method may not provide a total digest of all fertilizer samples.

ProcedureWeigh 1 g (0.5 g for organic matrices) of the sample into the digestion vessel. Add 9 mL of HNO₃, and 3 mL HCl. Gently swirl the mixture and wait approximately 20 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, with some particles (silicates) remaining upon dilution to 50 mL.

535

69

Microwave Digestion ofFertilizer - AOAC Method 2017.02

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Microwave Digestion ofFertilizer -AOAC Method 2006.03

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis method may not provide a total digest of all fertilizer samples.

ProcedureWeigh 1 g (0.5 g for organic matrices) of the sample into the digestion vessel. Add 10 ml of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

233

70

Microwave Digestion ofFertilizer - AOAC Method 2006.03

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Microwave Digestion ofFly Ash

EnvironmMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsH₂SO₄ H₃PO₄

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureAdd 0.1 g of the sample into the digestion vessel. Add 3 mL of H₂SO₄ and 3 mL of H₃PO₄. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 260 35:00 30:00 N/A 700-1800 Off

71

Microwave Digestion ofFly Ash in iPrep (Step 1 of 2)

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Microwave Digestion ofFly Ash

EnvironmMARS 6 (

ProcedureAllow vessels to cool. Open and add 1.5 mL of HNO₃, 1.5 mL of HCl, and 1.5 mL of HF. Wait approximately 15 minutes before closing the vessel.

Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

ReagentsHNO₃HClHF

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization". The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

649

72

Microwave Digestion ofFly Ash in iPrep (Step 2 of 2)

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Microwave Digestion ofLimestone

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesAllow any initial reaction to subside before sealing the vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve in soluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 7.5 mL of HNO₃ and 2.5 ml of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilutionto 50 ml.

2

73

Microwave Digestion ofLimestone

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Microwave Digestion ofNPDES (Waste Water)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeWater

Heating Program

Max Sample Weight50 mL

ReagentsHNO₃ HCl

Recommended Vessels75 mL MARSXpressEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 50 mL of the sample into the digestion vessel. Add 3 mL of HNO₃, and 2 mL HCl. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 165 30:00 0:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

252

74

Microwave Digestion ofNPDES (Waste Water)

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Microwave Digestion ofPine Needles

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃H₂O₂ (30%)

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 8 mL of HNO₃ and 2 mL of H₂O₂ (30%). Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

253

75

Microwave Digestion ofPine Needles

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Microwave Digestion ofRoHS (For Pb, Hg, and Cd Analysis)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃ H₂SO₄

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 10 mL of HNO₃, and 0.02 mL of H₂SO₄. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 10:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL

254

76

Microwave Digestion ofRoHS (For Pb, Hg, and Cd Analysis)

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Microwave Digestion ofSediment (BCCS - 1 CRM) (Leach)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis method may not provide a total digest of all samples. Hydrofluoric acid will be required to provide complete digestion of some sample matrixes. The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

255

77

Microwave Digestion ofSediment (BCCS - 1 CRM) (Leach)

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Microwave Digestion ofSediment (Buffalo River) (Leach)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis method may not provide a total digest of all samples. Hydrofluoric acid will be required to provide complete digestion of some sample matrixes. The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 175 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

256

78

Microwave Digestion ofSediment (Buffalo River) (Leach)

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Microwave Digestion ofSludge (Industrial)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe use of HF may be required to digest any silicates found in the sample. The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

257

79

Microwave Digestion ofSludge (Industrial)

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Microwave Digestion ofSoil (Montana - CRM) (Leach)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis method may not provide a total digest of all samples. Hydrofluoric acid will be required to provide complete digestion of some sample matrixes. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 175 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

258

80

Microwave Digestion ofSoil (Montana - CRM) (Leach)

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Microwave Digestion ofTCLP Extract

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeStandard Control

Sample TypeWater

Heating Program

Max Sample Weight25 mL

ReagentsHNO₃

Recommended VesselsEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 25 mL of the sample into the digestion vessel. Add 5 mL of HNO₃. Gently swirl the mixture before closing the vessel. If a high organic content is suspected, a 10 ml sample volume is recommended.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 10:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

259

81

Microwave Digestion ofTCLP Extract

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Microwave Digestion ofUS EPA 3015 (Aqueous Samples)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeStandard Control

Sample TypeWater

Heating Program

Max Sample Weight45 mL

ReagentsHNO₃

Recommended Vessels75 mL MARSXpressEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 45 mL of the sample into the digestion vessel. Add 5 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 10:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsThis method is intended to be an acid leach, not a total digest. Hydrofluoric acid will be required to provide complete digestion of the sample matrix.

260

82

Microwave Digestion ofUS EPA 3015 (Aqueous Samples)

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Microwave Digestion ofUS EPA 3015a (Aqueous Sample)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeStandard Control

Sample TypeWater

Heating Program

Max Sample Weight45 mL

ReagentsHNO₃HCl (Optional)

Recommended Vessels75 mL MARSXpressEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 45 mL of the sample into the digestion vessel. Add 5 mL of HNO3, or alternatively 4 mL of HNO₃ and 1 mL HCl. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 10:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsThis method is intended to be an acid leach, not a total digest. Hydrofluoric acid will be required to provide complete digestion of the sample matrix.

261

83

Microwave Digestion ofUS EPA 3015a (Aqueous Sample)

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Microwave Digestion ofUS EPA 3051 (Solid Sample)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeStandard Control

Sample TypeSolid

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl (Optional)

Recommended VesselsEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 175 5:30 4:30 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsThis method is intended to be an acid leach, not a total digest.

262

84

Microwave Digestion ofUS EPA 3051 (Solid Sample)

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Microwave Digestion ofUS EPA 3051a (Solid Sample)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeStandard Control

Sample TypeSolid

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl (Optional)

Recommended VesselsEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃, or alternatively 9 mL HNO₃, and 1 mL HCl. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 175 5:30 4:30 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsThis method is intended to be an acid leach, not a total digest.

263

85

Microwave Digestion ofUS EPA 3051a (Solid Sample)

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Microwave Digestion ofUS EPA 3052 (Sludge, Soil, Sediment or Oil)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeStandard Control

Sample TypeSolid

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 3 mL HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 5:30 9:30 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

264

86

Microwave Digestion ofUS EPA 3052 (Sludge, Soil, Sediment or Oil)

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Microwave Digestion ofUSP 232/233 (Pharmaceuticals)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL HCl. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

265

87

Microwave Digestion ofUSP 232/233 (Pharmaceuticals)

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Microwave Digestion ofWaste Activated Sludge

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃H₂O₂

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 5 mL of HNO₃, and 5 mL of H₂O₂. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

266

88

Microwave Digestion ofWaste Activated Sludge

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Microwave Digestion ofWater (For Analysis of Phosphorous)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeWater

Heating Program

Max Sample Weight50 mL

ReagentsK₂S₂O₈ H₂SO₄

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6

Notes

ProcedureTransfer 50 mL of H₂O into the digestion vessel. Add 0.5 g of K₂S₂O₈ and 1 mL of H₂SO₄. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

267

89

Microwave Digestion ofWater (For Analysis of Phosphorous)

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Microwave Digestion ofWood

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

268

90

Microwave Digestion ofWood

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Food Testing

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Microwave Digestion ofAlum

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 3 mL of HCl, 5 mL of HF, and 2 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain therequired results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at orbelow room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vesselsdetected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

536

92

Microwave Digestion ofAlum

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Microwave Digestion ofApple

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain therequired results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at orbelow room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vesselsdetected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

269

93

Microwave Digestion ofApple

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Microwave Digestion ofAsparagus

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Resultssample was clear, colorless, and particle free upon dilution to 50 mL.

270

94

Microwave Digestion ofAsparagus

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Microwave Digestion ofAspartame

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 15:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

758

95

Microwave Digestion ofAspartame in iPrep

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Microwave Digestion ofBacon (Cooked)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃DI H₂O

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1.0 g of the sample into the digestion vessel. Add 8 mL of HNO₃ and 2 mL of DI H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

271

96

Microwave Digestion ofBacon (Cooked)

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Microwave Digestion ofBeef (Ground)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1.0 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL

272

97

Microwave Digestion ofBeef (Ground)

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Microwave Digestion ofBeef Bouillon

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

537

98

Microwave Digestion ofBeef Bouillon

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Microwave Digestion ofBeer (Light)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight4 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 4 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

273

99

Microwave Digestion ofBeer (Light)

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Microwave Digestion ofBlueberry

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

275

100

Microwave Digestion ofBlueberry

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Microwave Digestion ofBroccoli

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 20 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

277

101

Microwave Digestion ofBroccoli

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Microwave Digestion ofCaramel Color

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2.0 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 2.0 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Resultssample was clear, colorless, and particle free upon dilution to 50 mL.

278

102

Microwave Digestion ofCaramel Color

Page 103: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofCarrot

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

279

103

Microwave Digestion ofCarrot

Page 104: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofCelery

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

280

104

Microwave Digestion ofCelery

Page 105: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofCheese (Cracker)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of ground sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

281

105

Microwave Digestion ofCheese (Cracker)

Page 106: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofCheese (Powder)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

538

106

Microwave Digestion ofCheese (Powder)

Page 107: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofCheese (Processed)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 ml of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

282

107

Microwave Digestion ofCheese (Processed)

Page 108: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofCherry

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

283

108

Microwave Digestion ofCherry

Page 109: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofChewing Gum

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis. The use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 ml.

284

109

Microwave Digestion ofChewing Gum

Page 110: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofChicken (Boneless)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

285

110

Microwave Digestion ofChicken (Boneless)

Page 111: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofChili Candy (Mexican)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

286

111

Microwave Digestion ofChili Candy (Mexican)

Page 112: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofChili Powder

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2 g

ReagentsHNO₃DI H₂O

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 2 g of the sample into the digestion vessel. Add 10 mL HNO₃ and 5 mL deionized H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and colorless with some small particles (silicates) remaining upon dilution to 50 mL.

680

112

Microwave Digestion ofChili Powder in iPrep

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Microwave Digestion ofChips (Potato)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

287

113

Microwave Digestion ofChips (Potato)

Page 114: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofCitrus Leaves

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃DI H₂OHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 6 mL of HNO₃, 3 mL of deionized H₂O, and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

539

114

Microwave Digestion ofCitrus Leaves

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Microwave Digestion ofClam Puree

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g (Wet Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1 g (wet weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

540

115

Microwave Digestion ofClam Puree

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Microwave Digestion ofCocoa

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

541

116

Microwave Digestion ofCocoa

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Microwave Digestion ofCoconut

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g (Wet Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1 g (wet weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

542

117

Microwave Digestion ofCoconut

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Microwave Digestion ofCoffee Beans

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may; however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of ground sample into the digestion vessel. Add 10 ml of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 ml.

10

118

Microwave Digestion ofCoffee Beans

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Microwave Digestion ofCucumber

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

289

119

Microwave Digestion ofCucumber

Page 120: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofDog Food

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of (dry weight) up to 1 g (wet weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 Ml

290

120

Microwave Digestion ofDog Food

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Microwave Digestion ofFish Tissue

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) up to 2 g (wet weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

543

121

Microwave Digestion ofFish Tissue

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Microwave Digestion ofFlounder

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2.0 g (Wet Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 2 g (wet weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

544

122

Microwave Digestion ofFlounder

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Microwave Digestion ofFlour

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

292

123

Microwave Digestion ofFlour

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Microwave Digestion ofFood

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g dry weight (0.25 g w/Xpress vessels) of the sample into the digestion vessel. Add 10 mL of HNO₃ . Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

294

124

Microwave Digestion ofFood

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Microwave Digestion ofFood Coloring (Liquid)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 mL.

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 0.5 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

293

125

Microwave Digestion ofFood Coloring (Liquid)

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Microwave Digestion ofFruit Juice

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2.5 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 2.5 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

295

126

Microwave Digestion ofFruit Juice

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Microwave Digestion ofGelatin

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

545

127

Microwave Digestion ofGelatin

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Microwave Digestion ofGranola Bar

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of ground sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

296

128

Microwave Digestion ofGranola Bar

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Microwave Digestion ofGrape

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

297

129

Microwave Digestion ofGrape

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Microwave Digestion ofGrapefruit

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

298

130

Microwave Digestion ofGrapefruit

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Microwave Digestion ofGummy Bear

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

729

131

Microwave Digestion ofGummy Bear

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Microwave Digestion ofHam

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1.0 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

299

132

Microwave Digestion ofHam

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Microwave Digestion ofInfant Cereal (Rice Grain)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

300

133

Microwave Digestion ofInfant Cereal (Rice Grain)

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Microwave Digestion ofInfant Formula (Liquid)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2 mL

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 2 mL of of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Results Sample was clear, colorless and particle free upon dilution to 50 mL

301

134

Microwave Digestion ofInfant Formula (Liquid) in iPrep

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Microwave Digestion ofInfant Formula (Liquid)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 1 mL (0.5 mL w/Xpress Vessels) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

302

135

Microwave Digestion ofInfant Formula (Liquid)

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Microwave Digestion ofInfant Formula (Powder)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

303

136

Microwave Digestion ofInfant Formula (Powder) in iPrep

Page 137: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofInfant Formula (Powder)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

304

137

Microwave Digestion ofInfant Formula (Powder)

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Microwave Digestion ofKidney Bean

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

305

138

Microwave Digestion ofKidney Bean

Page 139: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofKielbasa Sausage

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g (Wet Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1 g (wet weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

546

139

Microwave Digestion ofKielbasa Sausage

Page 140: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofMaple Syrup

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

306

140

Microwave Digestion ofMaple Syrup

Page 141: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofMayonnaise

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

307

141

Microwave Digestion ofMayonnaise

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Microwave Digestion ofMeal Replacement Shake (Chocolate)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Mix)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry mix) of the sample into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

547

142

Microwave Digestion ofMeal Replacement Shake (Chocolate)

Page 143: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofMilk (Whole - Liquid)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight4 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 4 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

309

143

Microwave Digestion ofMilk (Whole - Liquid)

Page 144: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofMilk (Powder)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

310

144

Microwave Digestion ofMilk (Powder)

Page 145: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofNutritional Drink (Adult)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 1.0 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

276

145

Microwave Digestion ofNutritional Drink (Adult)

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Microwave Digestion ofOlive Oil

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

312

146

Microwave Digestion ofOlive Oil

Page 147: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofOrange Juice

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2.5 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 2.5 ml of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

313

147

Microwave Digestion ofOrange Juice

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Microwave Digestion ofOyster Puree

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g (Wet Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1 g (wet weight) of the sample into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

548

148

Microwave Digestion ofOyster Puree

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Microwave Digestion ofPeanut Butter

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

314

149

Microwave Digestion ofPeanut Butter

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Microwave Digestion ofPear

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

315

150

Microwave Digestion ofPear

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Microwave Digestion ofPepper (Bell, Chili, Etc.)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

316

151

Microwave Digestion ofPepper (Bell, Chili, Etc.)

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Microwave Digestion ofPistachio Nuts

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

549

152

Microwave Digestion ofPistachio Nuts

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Microwave Digestion ofPizza (Frozen, Pepperoni)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1.0 g (homogenized) into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Resultssample was clear, colorless, and particle free upon dilution to 50 mL.

317

153

Microwave Digestion ofPizza (Frozen, Pepperoni)

Page 154: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofPlum

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

318

154

Microwave Digestion ofPlum

Page 155: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofPork (Ground)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 2.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

319

155

Microwave Digestion ofPork (Ground)

Page 156: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofPotato

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

320

156

Microwave Digestion ofPotato

Page 157: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofPotato Chips

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Ground)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (ground) of the sample into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

550

157

Microwave Digestion ofPotato Chips

Page 158: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofPretzel (Salted)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

321

158

Microwave Digestion ofPretzel (Salted)

Page 159: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofProtein Bar

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

322

159

Microwave Digestion ofProtein Bar

Page 160: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofRaspberry

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

323

160

Microwave Digestion ofRaspberry

Page 161: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofRice

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

324

161

Microwave Digestion ofRice

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Microwave Digestion ofSafflower Oil

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

325

162

Microwave Digestion ofSafflower Oil

Page 163: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofSalad Dressing (Ranch)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Mix)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry mix) of the sample into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

551

163

Microwave Digestion ofSalad Dressing (Ranch)

Page 164: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofSalami

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

326

164

Microwave Digestion ofSalami

Page 165: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofSausage

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

327

165

Microwave Digestion ofSausage

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Microwave Digestion ofSoda (Diet)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight 1 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 1 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

328

166

Microwave Digestion ofSoda (Diet)

Page 167: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofSodium Free - Seasoning

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

552

167

Microwave Digestion ofSodium Free - Seasoning

Page 168: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofSoybean

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of (dry weight) sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

235

168

Microwave Digestion ofSoybean

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Microwave Digestion ofSpinach

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

331

169

Microwave Digestion ofSpinach

Page 170: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

Microwave Digestion ofSpinach Leaves

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis. Some plant tissues contain silicates which would require HF for total dissolution.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

330

170

Microwave Digestion ofSpinach Leaves

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Microwave Digestion ofSpinach Pasta

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

553

171

Microwave Digestion ofSpinach Pasta

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Microwave Digestion ofStrawberry

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

332

172

Microwave Digestion ofStrawberry

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Microwave Digestion ofSugar (Granulated)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

333

173

Microwave Digestion ofSugar (Granulated)

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Microwave Digestion ofTea (Chai)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2.5 g

ReagentsHNO₃ DI H₂O

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 2.5 g of the sample into the digestion vessel. Add 10 mL HNO₃ and 5 mL deionized H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and colorless with some small particles (silicates) remaining upon dilution to 50 mL.

679

174

Microwave Digestion ofTea (Chai) in iPrep

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Microwave Digestion ofTea Leaves

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

334

175

Microwave Digestion ofTea Leaves

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Microwave Digestion ofTomato Leaves

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesSome plant tissues contain silicates which would require HF for total dissolution.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, with white silica particles upon dilution to 50 mL.

335

176

Microwave Digestion ofTomato Leaves

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Microwave Digestion ofTomato Paste (70% Moisture)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 2 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

554

177

Microwave Digestion ofTomato Paste (70% Moisture)

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Microwave Digestion ofTomato Soup

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight5 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 5 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

336

178

Microwave Digestion ofTomato Soup

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Microwave Digestion ofWalnut

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

337

179

Microwave Digestion ofWalnut

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Microwave Digestion ofWatermelon

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

338

180

Microwave Digestion ofWatermelon

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Microwave Digestion ofWheat Crackers

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

555

181

Microwave Digestion ofWheat Crackers

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Microwave Digestion ofWhey

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

340

182

Microwave Digestion ofWhey

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Microwave Digestion ofWhey (Powder)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

339

183

Microwave Digestion ofWhey (Powder)

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Microwave Digestion ofWine

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 1 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

341

184

Microwave Digestion ofWine

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Microwave Digestion ofYogurt (Plain)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1.0 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

342

185

Microwave Digestion ofYogurt (Plain)

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Geoscience & Mining

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187

Microwave Digestion ofAlpha - Alumina

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeHCl

Heating Program

Max Sample Weight0.5 g

ReagentsHCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The maximum number of vessels that can be run for this method is 6.

Ensure that particles are well suspended in acid mixture prior to sealing vessel.

Stirring may be helpful to keep particles suspended in solution during digestion.

ProcedureWeigh 0.5 g of sample into the digestion vessel. Add 10 mL HCl. Gently swirl the vessel to thoroughly mix the sample and acid.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 59:59 N/A 900-1800 N/A

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain therequired results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at orbelow room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vesselsdetected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

343

Microwave Digestion ofAlpha - Alumina in iPrep

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188

Microwave Digestion ofAlumina Beads (w/ Silver substrate)

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsH₃PO₄H₂SO₄

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 6.5 mL of H₃PO₄, and 3.5 mL of H₂SO₄. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 280 30:00 45:00 N/A 700-1800 Off

Microwave Digestion ofAlumina Beads (with Silver Substrate) in iPrep (Step 1 of 2)

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189

Microwave Digestion ofAlumina Beads (w/ Silver substrate)

GeoscienMARS 6 (

ProcedureAllow vessel to cool after completion of Step 1. Proceeding step one, add 3 mL of HNO₃, and 3 mL HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

ReagentsHNO₃HF

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 25:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL

616

Microwave Digestion ofAlumina Beads (with Silver Substrate) (Step 2 of 2)

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190

Microwave Digestion ofAlumina Powder

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsH₃PO₄

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureAdd 0.1 g of the sample into the digestion vessel. Add 8 mL of H₃PO₄. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 275 30:00 45:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, gold colored, and particle free upon dilution to 50 mL.

672

Microwave Digestion ofAlumina Powder in iPrep

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191

Microwave Digestion ofAluminum Nitride

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsH₃PO₄ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 5 mL H₃PO₄ and 10 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 175 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

560

Microwave Digestion ofAluminum Nitride

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192

Microwave Digestion ofAluminum Oxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsH₃PO₄H₂SO₄

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesEasyPrep Plus requires a high temperature probe for this method.

Ensure that particles are well suspended in acid mixture prior to sealing vessel.

Stirring may be helpful to keep particles suspended in solution during digestion.

ProcedureWeigh 0.25 g of sample into the digestion vessel. Add 6.5 mL H₃PO₄ and 3.5 mL H₂SO₄. Gently swirl the vessel to thoroughly mix the sample and acid.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 270 30:00 20:00 N/A 900-1800 N/A

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

344

Microwave Digestion ofAluminum Oxide

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193

Microwave Digestion ofAluminum Oxide (H₃PO₄)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1g

ReagentsH₃PO₄

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This method may not provide a total digest of all samples. Hydrofluoric acid may be required to provide complete digestion of some sample matrixes.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 8 mL H₃PO₄. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 260 25:00 45:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and colorless with some white particles remaining upon dilution to 50 mL.

673

Microwave Digestion ofAluminum Oxide (H3PO4) in iPrep

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194

Microwave Digestion ofAsbestos

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsHClHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesHF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 6 mL of HCl, 3 mL of HNO₃, and 3 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

492

Microwave Digestion ofAsbestos

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195

Microwave Digestion ofAutomotive Catalyst

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.4 g

ReagentsHClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. Reducing the particle size increases the efficiency of digestion and may decrease the digestion time.

ProcedureWeigh 0.4 g of the sample into the digestion vessel. Add 10 mL of HCl and 0.5 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

345

Microwave Digestion ofAutomotive Catalyst

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196

Microwave Digestion ofBarium Titanate (BaTiO₃)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesHF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel. This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 5 mL of HNO3 and 10 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

493

Microwave Digestion ofBarium Titanate (BaTiO3)

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197

Microwave Digestion ofBastnaesite Ore

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHClHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

This method could potentially form HF. It is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 9 mL of HCl and 3 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 30:00 800 900-1800 Off

Microwave Digestion ofBastnaesite Ore (Step 1 of 2)

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198

Microwave Digestion ofBastnaesite Ore

GeoscienMARS 6 (

ProcedureAllow vessels to cool. Open and add 1 g solid Boric Acid and 20 mL deionized H₂O. Wait approximately 15 minutes before closing the vessel.

ReagentsSolid Boric AcidDI H₂O

Notes

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 175 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

559

Microwave Digestion ofBastnaesite Ore (Step 2 of 2)

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199

Microwave Digestion ofBauxite

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsH₃PO₄ H₂SO₄

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 6.5 mL of H₃PO₄ and 3.5 mL of H₂SO₄. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 15:00 15:00 800 900-1800 Off

Microwave Digestion ofBauxite (Step 1 of 2)

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200

Microwave Digestion ofBauxite

GeoscienMARS 6 (

ProcedureProceeding step 1 add 1 mL of HNO₃, 1 mL of HCl, and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

ReagentsHNO₃HClHF

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL

599

Microwave Digestion ofBauxite (Step 2 of 2)

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201

Microwave Digestion ofBismuth Aluminate Mixture

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHClHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 9 mL HCl and 3 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 190 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon diltuion to 50 mL.

746

Microwave Digestion ofBismuth Aluminate Mixture

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202

Microwave Digestion ofBismuth Yttrium Iron Oxide

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeHCl

Heating Program

Max Sample Weight0.1 g

ReagentsHCLHNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

HF should be added slowly and carefully to the sample.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 6 mL of HCl, 2 mL of HNO₃, and 0.5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 25:00 15:00 N/A 700-1800 Off

Microwave Digestion ofBismuth Yttrium Iron Oxide in iPrep (Step 1 of 2)

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203

Microwave Digestion ofBismuth Yttrium Iron Oxide

GeoscienMARS 6 (

ProcedureAllow vessel to cool. Add 1.75 g of solid H₃BO₃ + 20 mL deionized H₂O into the vessel that contains the sample and acid.

ReagentsSolid H₃BO₃DI H₂O

NotesThis procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction of certain analytes with hydrofluoric acid.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeStandard

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 25:00 10:00 N/A 700-1800 Off

General Precautiona) If using HF, follow restrictions listed in HF Addendum.b) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, yellow in color, and particle free upon dilution to 50 mL.

743

Microwave Digestion ofBismuth Yttrium Iron Oxide in iPrep (Step 2 of 2)

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204

Microwave Digestion ofBoiler Scale (80-90% Fe)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 5 mL of HNO₃ and 5 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

494

Microwave Digestion ofBoiler Scale (80-90% Fe)

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205

Microwave Digestion ofBoric Acid HF Neutralization

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample WeightVaries by Sample

ReagentsH₃BO₃ (4%)

Recommended VesselsEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction of certain analytes with hydrofluoric acid.

Alternatively, 1-4 g of solid H₃BO₃ + 25 mL deionized H₂O can be used in place of the 4% w/v solution.

ProcedureAllow vessel to cool. Add 30 mL H₃BO₃ (4%) into the vessel that contains the sample and acid.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSee sample specific method notes.

6

Microwave Digestion ofBoric Acid HF Neutralization

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206

Microwave Digestion ofBoron Carbide (B₄C)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃H₂SO₄HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “BoricAcid HF Neutralization”.

Reducing the particle size increases the efficiency of digestion and may decrease the digestion time.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 5 mL of HNO₃ and 5 mL of H₂SO₄. Gently swirl to mix the sample particles in the acid. Slowly and carefully add 5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 270 30:00 30:00 800 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

674

Microwave Digestion ofBoron Carbide (B4C) in iPrep

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207

Microwave Digestion ofCarbon

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe structure, form and surface area of carbon samples varies widely. Higher temperatures and use of other reagents may be necessary in order to digest certain samples.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 10 mL of HNO₃ . Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 215 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

348

Microwave Digestion ofCarbon

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208

Microwave Digestion ofCement

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsHNO₃HClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 3 mL of HNO₃ , 6 mL of HCL, and 3 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 175 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

349

Microwave Digestion ofCement

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209

Microwave Digestion ofCeramic (Fused Silica)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesHF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing the vessel. This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Slowly add 2 mL of HNO₃ , and 8 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 190 10:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

350

Microwave Digestion ofCeramic (Fused Silica)

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210

Microwave Digestion ofCeramics

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0. 2 g of the sample into the digestion vessel. Add 5 mL of HNO₃ , and 5 ml of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

351

Microwave Digestion ofCeramics

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211

Microwave Digestion ofChar - Sulfuric Acid

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample WeightVaries by sample

ReagentsH₂SO₄

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesEasyPrep Plus requires a high temperature probe for this method. This method is for the pretreatment of large sample sizes or difficult organic samples that are resistant to oxidation. After the char is complete, the vessel is opened and a normal oxidation with HNO₃ can be run, usually at around 200C.

ProcedureAdd 6 mL H₂SO₄ into the vessel that contains the sample and acid.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 260 15:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSee sample specific method notes.

352

Microwave Digestion ofChar - Sulfuric Acid

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212

Microwave Digestion ofChromium Carbide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃ and 10 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

558

Microwave Digestion ofChromium Carbide

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213

Microwave Digestion ofChromium Oxide (Cr₂O₃)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeStandard

Heating Program

Max Sample Weight50 mg

ReagentsH₂SO₄HNO₃H₂O₂ (30%)

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

Stirring is required for complete dissolution of this sample type.

ProcedureWeigh 50 mg of the sample into the digestion vessel. Insert stir bar into the vessel. Add 4.5 mL of H₂SO₄ and 4 mL of HNO₃ to the vessel, then 1.5 mL of H₂O₂ (30%) dropwise. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 280 30:00 59:59 N/A 900-1800 Med

2 280 0:00 30:01 N/A 900-1800 Med

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and turquoise colored upon dilution to 50 mL.

681

Microwave Digestion ofChromium Oxide (Cr2O3) in iPrep

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214

Microwave Digestion ofClay

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHFHNO₃HCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

The addition of Conc. HCl (0-4 Ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 3 mL of HNO₃ , 1 mL of HCl, and 5 ml of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

353

Microwave Digestion ofClay

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215

Microwave Digestion ofCoal

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel. The use of HF may be required to digest any silicates found in the sample. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 250 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless with some particles remaining upon dilution to 50 mL.

355

Microwave Digestion ofCoal in iPrep

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216

Microwave Digestion ofCoal

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe use of HF may be required to digest any silicates found in the sample. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

356

Microwave Digestion ofCoal

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217

Microwave Digestion ofCoal Ash

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsHNO₃HClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 3 mL of HNO₃ , 3 mL of HCl and 3 ml of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

354

Microwave Digestion ofCoal Ash

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218

Microwave Digestion ofCryolite / Electrolytic Bath

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesCryolite / Electrolytic Bath is approximately 55% Cryolite (Na₃AlF₆) and 30% Chiolite (Na₅Al₃F₁₄).

ProcedureWeigh 0.5g of the sample into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

Microwave Digestion ofCryolite / Electrolytic Bath (Step 1 of 2)

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219

Microwave Digestion ofCryolite / Electrolytic Bath

GeoscienMARS 6 (

ProcedureAllow vessel to cool after completion of Step 1. Open and add 30 mL of Deionized Water and 2 g Boric Acid (solid). Gently swirl the mixture and seal the vessel.

ReagentsDI H₂OBoric Acid (solid)

Notes

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 175 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

496

Microwave Digestion ofCryolite / Electrolytic Bath (Step 2 of 2)

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220

Microwave Digestion ofFeldspar

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHCl HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel. This procedure uses hydrofluoric acid. It is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 2 mL of HCl and 8 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 30:00 25:00 N/A 700-1800 Off

Microwave Digestion ofFeldspar in iPrep (Step 1 of 2)

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221

Microwave Digestion ofFeldspar

GeoscienMARS 6 (

ProcedureAllow vessels to cool. Open and add 4 g solid boric acid and 30 mL of deionized H2O. Wait approximately 15 minutes before closing the vessel.

ReagentsSolid Boric AcidDI H₂O

Notes

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 30:00 10:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

647

Microwave Digestion ofFeldspar (Step 2 of 2)

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222

Microwave Digestion ofFerric Oxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHClHNO₃DI H₂O

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 10 mL of a 1:1:1 HCl, HNO₃, and Deionized H₂O mixture. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 25:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, yellow in color, and particle free upon dilution to 50 mL.

744

Microwave Digestion ofFerric Oxide in iPrep

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223

Microwave Digestion ofFurnace Slag

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureAdd 0.5 g of the sample into the digestion vessel. Add 3 mL of HNO₃, 2 mL of HCl, and 5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

498

Microwave Digestion ofFurnace Slag

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224

Microwave Digestion ofGadolinium Zirconium Oxide

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeStandard

Heating Program

Max Sample Weight0.1 g

ReagentsH₂SO₄HNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

HF should be added slowly and carefully to the sample.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 4 mL of H₂SO₄, 1.5 mL of HNO₃ and 1.5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 280 35:00 30:00 N/A 700-1800 High

Microwave Digestion ofGadolinium Zirconium Oxide in iPrep (Step 1 of 2)

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225

Microwave Digestion ofGadolinium Zirconium Oxide

GeoscienMARS 6 (

ProcedureAllow vessel to cool. Add 1.5 g of solid H₃BO₃ + 20 mL deionized H₂O into the vessel that contains the sample and acid.

ReagentsH₃BO₃DI H₂O

NotesThis procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction of certain analytes with hydrofluoric acid.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeStandard

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 25:00 10:00 N/A 700-1800 High

General Precautiona) If using HF, follow restrictions listed in HF Addendum.b) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

742

Microwave Digestion ofGadolinium Zirconium Oxide in iPrep (Step 2 of 2)

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226

Microwave Digestion ofGas Atomized Powder

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HClHF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 8 mL of HNO₃, 2 mL of HCl, and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSamples were clear, green in color and particle free upon dilution to 50 mL.

721

Microwave Digestion ofGas Atomized Powder in iPrep

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227

Microwave Digestion ofGlass Fiber

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.4 g

ReagentsHNO₃HClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureAdd 0.4 g of the sample into the digestion vessel. Add 2 mL of HNO₃, 4 mL of HCl, and 4 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

499

Microwave Digestion ofGlass Fiber

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228

Microwave Digestion ofHafnium Oxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HCl or H₂OHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel. HNO3:HF:H2O (1:1:1) can be substituted for HNO3:HCl:HF (1:1:1) using the same heating program if the use of HCl is not desired. Mixtures are made from acids in their concentrated form.

ProcedureAdd 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃:HCl:HF (1:1:1) or alternatively, HNO₃:H₂O:HF (1:1:1). (See Notes) Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

500

Microwave Digestion ofHafnium Oxide

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229

Microwave Digestion ofIlmenite (FeTiO₃)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 5 mL of HNO₃, 1 mL of HCl, and 10 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

501

Microwave Digestion ofIlmenite (FeTiO3)

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230

Microwave Digestion ofIron Ore

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsH₂OHClHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization” The addition of Conc. HCl (0-8 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 g of the sample into the digestion vessel. Add 4 mL of H₂O, 8 ml of HCl, 4 mL of HNO₃, and 4 mL of HF. Gently swirl the mixture and wait approximately 15 minute before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

358

Microwave Digestion ofIron Ore

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231

Microwave Digestion ofKaolin

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHClHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 3 mL of HCl, 1 mL of HNO3, and 7 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

502

Microwave Digestion ofKaolin

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232

Microwave Digestion ofKerosene

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe pre-digestion step will allow the lighter fuel fractions to react before sealing the vessels.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

359

Microwave Digestion ofKerosene

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233

Microwave Digestion ofLead Sulfide (PbS)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 5 mL of HNO₃ and 5 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

503

Microwave Digestion ofLead Sulfide (PbS)

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234

Microwave Digestion ofLithium Nickel Cobalt Manganese Oxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HCl

Recommended VesselsMARSXpress

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 4 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 10:00 N/A 1030-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsThe samples were clear, green in color, and particle free upon dilution.

724

Microwave Digestion ofLithium Nickel Cobalt Manganese Oxide

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235

Microwave Digestion ofMagnesium Oxide (MgO 40 -54 %)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsH₂O (deionized)HClHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution.The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 5 mL of DI H₂O, 5 mL HCl, and 5 mL HNO₃. Gently swirl and allow approximately 15 minutes for pre-digestion.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

762

Microwave Digestion ofMagnesium Oxide (MgO 40-54%)

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236

Microwave Digestion ofManganous Oxide (MnO)

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.2g of the sample into the digestion vessel. Add 10 mL HNO₃ and 3 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 10:00 800 900-1800 Off

Microwave Digestion ofManganous Oxide (MnO) (Step 1 of 2)

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237

Microwave Digestion ofManganous Oxide (MnO)

GeoscienMARS 6 (

ProcedureAllow vessel to cool after completion of Step 1. Open and add 5 mL of HCl. Gently swirl the mixture and seal the vessel.

ReagentsHCl

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

505

Microwave Digestion ofManganous Oxide (MnO) (Step 2 of 2)

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238

Microwave Digestion ofMica

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsH₃PO₄HClHF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 4 mL of H₃PO₄, 3 mL of HCl, and 0.5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

690

Microwave Digestion ofMica in iPrep

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239

Microwave Digestion ofMill Tailings

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsH₃PO₄H₂SO₄

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesEasyPrep Plus vessels require a high temperature probe for this method.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 3 mL of H₃PO₄, and 2 mL of H₂SO₄. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 270 15:00 30:00 800 900-1800 Off

Microwave Digestion ofMill Tailings (Step 1 of 2)

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240

Microwave Digestion ofMill Tailings

GeoscienMARS 6 (

ProcedureCool, vent and open vessel after step 1. Add 2.5 mL HNO₃, 2.5 mL HCl, 2.5 mL HF, and 2.5 ml H₂O. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing the vessel.

ReagentsHNO₃HClHFH₂O

NotesThe above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in method note entitled “Boric HF Neutralization” The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

600

Microwave Digestion ofMill Tailings (Step 2 of 2)

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241

Microwave Digestion ofMineral Ore

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsHNO₃ HClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 3 mL of HNO₃, 3 mL of HCl, and 3 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 10:00 800 900-1800 Off

Microwave Digestion ofMineral Ore (Step 1 of 2)

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242

Microwave Digestion ofMineral Ore

GeoscienMARS 6 (

ProcedureProceeding step 1 add 25 mL of Boric Acid (4%). Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

ReagentsH₃BO₃ (4%)

Notes

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL

516

Microwave Digestion ofMineral Ore (Step 2 of 2)

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243

Microwave Digestion ofMolybdenum Disulfide (MoS₂)

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureAdd 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

Microwave Digestion ofMolybdenum Disulfide (MoS2) (Step 1 of 2)

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244

Microwave Digestion ofMolybdenum Disulfide (MoS₂)

GeoscienMARS 6 (

ProcedureAllow vessel to cool after completion of Step 1. Add 10 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

ReagentsHCl

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 10:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

506

Microwave Digestion ofMolybdenum Disulfide (MoS2) (Step 2 of 2)

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245

Microwave Digestion ofNickel (II) Hydroxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HCl

Recommended VesselsMARSXpress

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 4 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 10:00 N/A 1030-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsThe samples were clear, light green in color, and particle free upon dilution.

725

Microwave Digestion ofNickel (II) Hydroxide

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246

Microwave Digestion ofNiobium Pentoxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureAdd 1.0 g of the sample into the digestion vessel. Add 2 mL of HNO₃, and 10 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

508

Microwave Digestion ofNiobium Pentoxide

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247

Microwave Digestion ofPetroleum Coke

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsH₂SO₄

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 10 mL of H₂SO₄. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 260 15:00 15:00 800 900-1800 Off

Microwave Digestion ofPetroleum Coke (Step 1 of 2)

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248

Microwave Digestion ofPetroleum Coke

GeoscienMARS 6 (

ProcedureProceeding step 1 add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

ReagentsHNO₃

Notes

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL

601

Microwave Digestion ofPetroleum Coke (Step 2 of 2)

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249

Microwave Digestion ofPhosphate (21%)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsH₂O₂ (30%)HClHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 5 mL of H₂O₂ (30%), 5 mL HCl dropwise (wait for reaction to subside before adding next acid), and 5 mL HNO₃. Gently swirl the mixture and wait approximately 1 hour before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

761

Microwave Digestion ofPhosphate (21%)

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250

Microwave Digestion ofPhosphate Rock

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HBF₄

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureAdd 0.5 g of the sample into the digestion vessel. Add 5 mL of HNO₃, 5 mL of HBF₄. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

509

Microwave Digestion ofPhosphate Rock

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251

Microwave Digestion ofPollucite Ore

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃ HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 3 mL of HNO₃ and 5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 25:00 25:00 N/A 700-1800 Off

Microwave Digestion ofPollucite Ore in iPrep (Step 1 of 2)

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252

Microwave Digestion ofPollucite Ore

GeoscienMARS 6 (

ProcedureAllow vessel to cool. Add 2.5 g H₃BO₃ and 25 mL of deionized H₂O into the vessel that contains the sample and acid.

ReagentsH₃BO₃ DI H₂O

NotesThis procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction of certain analytes with hydrofluoric acid.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 25:00 15:00 N/A 700-1800 Off

General Precautiona) If using HF, follow restrictions listed in HF Addendum.b) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.c) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and particle free upon dilution to 50 mL.

757

Microwave Digestion ofPollucite Ore in iPrep (Step 2 of 2)

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253

Microwave Digestion ofPyrophyllite (AlSi₂)5(OH)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureAdd 0.25 g of the sample into the digestion vessel. Add 3 mL of HNO₃, 1 mL of HCl, and 7 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

510

Microwave Digestion ofPyrophyllite (AlSi2)5(OH)

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254

Microwave Digestion ofQuartz Powder

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 1 g of the sample into the digestion vessel. Add 10 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

511

Microwave Digestion ofQuartz Powder

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255

Microwave Digestion ofRock (Pulverized)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHClHFHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 5 mL of HNO₃, 3 mL of HCl, and 3 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

361

Microwave Digestion ofRock (Pulverized)

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256

Microwave Digestion ofRock, High Sulfide

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 30:00 15:00 N/A 700-1800 Off

Microwave Digestion ofRock, High Sulfide in iPrep (Step 1 of 2)

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257

Microwave Digestion ofRock, High Sulfide

GeoscienMARS 6 (

ProcedureProceeding step 1 add 3 mL of HF, and 2 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

ReagentsHFHCl

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 25:00 10:00 N/A 700-1800 Off

General Precautiona) If using HF, follow restrictions listed in HF Addendum.b) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.c) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.d) The control / reference vessel must contain the largest and most reactive sample.e) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL

628

Microwave Digestion ofRock, High Sulfide in iPrep (Step 2 of 2)

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258

Microwave Digestion ofRutile Ore

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HF H₃PO₄.

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization”

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 4 mL of HNO₃, 3 mL of H₃PO₄, and 8 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 15:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 ml.

362

Microwave Digestion ofRutile Ore

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259

Microwave Digestion ofSand

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HFHCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization” The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 3 mL of HNO₃, 2 mL of HCl, and 5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

363

Microwave Digestion ofSand

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260

Microwave Digestion ofShale

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHFHNO₃HCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.5 g of sample into the digestion vessel. Add 7 mL of HF, 3 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 25:00 15:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

698

Microwave Digestion ofShale in iPrep

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261

Microwave Digestion ofSilica Sand

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsH₂OHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesAdd HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides. The above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization” Reducing the particle size increase the efficiency of digestion and may decrease the digestion time.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 5 mL of H₂O, 3 mL of HNO₃, and 8 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

364

Microwave Digestion ofSilica Sand

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262

Microwave Digestion ofSilica Sand

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHClHF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 2 mL of HCl and 8 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 30:00 25:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsThe sample was clear, colorless and particle free upon dilution to 50 mL.

700

Microwave Digestion ofSilica Sand in iPrep

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263

Microwave Digestion ofSilicon Dioxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesAdd HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides. The above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization” Reducing the particle size increase the efficiency of digestion and may decrease the digestion time.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 2 mL of HNO₃, and 8 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 10:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

365

Microwave Digestion ofSilicon Dioxide

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264

Microwave Digestion ofSilicon Nitride

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureAdd 0.1 g of the sample into the digestion vessel. Add 1 mL of HNO₃ and 5 mL HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

701

Microwave Digestion ofSilicon Nitride in iPrep

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265

Microwave Digestion ofSilicon Wafer

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Piece (Approx 0.5 g)

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureAdd 1 piece (approx. 0.5 g) of the sample into the digestion vessel. Add 6 mL of HF and 3 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 10:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

366

Microwave Digestion ofSilicon Wafer

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266

Microwave Digestion ofSlag - Furnace

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization” The addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 3 mL of HNO₃, 5 mL of HCl, and 5 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

367

Microwave Digestion ofSlag - Furnace

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267

Microwave Digestion ofSodium Antimonate

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHClHNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.5 g of sample into the digestion vessel. Add 10 mL of HCl, 3 mL of HNO₃, and 2 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 30:00 15:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

702

Microwave Digestion ofSodium Antimonate in iPrep

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268

Microwave Digestion ofSpodumene (Lithium Feldspar)

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHClHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh .25 g of the sample into the digestion vessel. Add 3 mL of HCl, 1 mL of HNO₃ and 4 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 20:00 800 900-1800 Off

Microwave Digestion ofSpodumene (Lithium Feldspar) (Step 1 of 2)

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269

Microwave Digestion ofSpodumene (Lithium Feldspar)

GeoscienMARS 6 (

ProcedureAllow vessel to cool after completion of Step 1. Open and add 30 mL of Deionized H₂O and 2 g H₃BO₃ (solid). Gently swirl the mixture and seal the vessel.

ReagentsDeionized H₂OH₃BO₃ (solid)

Notes

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

512

Microwave Digestion ofSpodumene (Lithium Feldspar) (Step 2 of 2)

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270

Microwave Digestion ofSulfide Bulk Concentrate

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 30:00 20:00 N/A 700-1800 Off

Microwave Digestion ofSulfide Bulk Concentrate in iPrep (Step 1 of 2)

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271

Microwave Digestion ofSulfide Bulk Concentrate

GeoscienMARS 6 (

ProcedureProceeding step 1 add 5 mL of HCl, and 5 mL of Deionized Water. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

ReagentsHClDI H₂O

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 30:00 10:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL

635

Microwave Digestion ofSulfide Bulk Concentrate in iPrep (Step 2 of 2)

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272

Microwave Digestion ofTantalum Pentoxide (Ta₂O₅)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of sample into the digestion vessel. Add 3 mL of HNO₃, and 7 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 25:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

707

Microwave Digestion ofTantalum Pentoxide (Ta2O5) in iPrep

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273

Microwave Digestion ofTitanium Dioxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃ and 2 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

489

Microwave Digestion ofTitanium Dioxide

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274

Microwave Digestion ofTitanium Slag Ore

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.25 g of sample into the digestion vessel. Add 5 mL of HNO₃, and 10 mL of HF. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing the vessel.

Reducing the particle size increases the efficiency of digestion and may decrease the digestion time.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

708

Microwave Digestion ofTitanium Slag Ore in iPrep

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275

Microwave Digestion ofTungsten Carbide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesAdd HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides. The above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization” Reducing the particle size increase the efficiency of digestion and may decrease the digestion time.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Slowly add 5 mL of HNO₃, and 10 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 20:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

369

Microwave Digestion ofTungsten Carbide

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276

Microwave Digestion ofTungsten Ore (50% W; 10% Fe; 2% Mn)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 9 mL of HCl and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 25:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

513

Microwave Digestion ofTungsten Ore (50% W; 10% Fe; 2% Mn)

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277

Microwave Digestion ofTungsten Oxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesAdd HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides. The above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization” Reducing the particle size increase the efficiency of digestion and may decrease the digestion time.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Slowly add 2 mL of HNO₃, and 7 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 20:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

370

Microwave Digestion ofTungsten Oxide

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278

Microwave Digestion ofVermiculite

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureAdd 0.25 g of the sample into the digestion vessel. Add 1 mL of HNO₃, 4 mL of HCl, and 10 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

514

Microwave Digestion ofVermiculite

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279

Microwave Digestion ofWollastonite (Calcium Silicate)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsH₃PO₄HNO₃HBF₄

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.1 g of sample into the digestion vessel. Add 3 mL of H₃PO₄, 2 mL of HNO₃, and 3 mL of HBF₄. HBF₄ should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

711

Microwave Digestion ofWollastonite (Calcium Silicate) in iPrep

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280

Microwave Digestion ofZeolite

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesAdd HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides. The above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization”

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 5 mL of HNO₃, 4 mL of HCl, and 2 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

371

Microwave Digestion ofZeolite

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281

Microwave Digestion ofZinc Oxide (ZnO)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 5 mL of HNO₃ and 2 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

393

Microwave Digestion ofZinc Oxide (ZnO)

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282

Microwave Digestion ofZinc Oxide (ZnO)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.25 g of the sample (onto a filter disk) into the digestion vessel. Add 5 mL HNO₃ and 2 mL HF. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 25:00 15:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

712

Microwave Digestion ofZinc Oxide (ZnO) in iPrep

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283

Microwave Digestion ofZircon

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight50 mg

ReagentsH₂SO₄HNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureAdd 50 mg of the sample into the digestion vessel. Add 4 mL of H₂SO₄, 1.5 mL of HNO₃, and 1.5 mL HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 270 40:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

713

Microwave Digestion ofZircon in iPrep

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Industrial Hygiene

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285

Microwave Digestion ofAsbestos

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsHClHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesHF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 6 mL of HCl, 3 mL of HNO₃, and 3 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

492

Microwave Digestion ofAsbestos

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286

Microwave Digestion ofFilter (MCE)

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight60 mg

ReagentsHClHNO₃

Recommended Vessels20 mL MARSXpress

Recommended EquipmentMARS 6 iWave

NotesThis method was completed in the 20 mL disposable liner.

ProcedureWeigh one 37mm filter and one 25 mm filter (60 mg total) into the digestion vessel. Add 1 mL of HCl and 1 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 20:00 10:00 N/A 1050-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

745

Microwave Digestion ofFilter (MCE)

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287

Microwave Digestion ofFilter Paper - 37 mm Mixed Cellulose Ester

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Filter (Approx 0.3 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 filter (approx 0.3 g) into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

373

Microwave Digestion ofFilter Paper - 37 mm Mixed Cellulose Ester

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288

Microwave Digestion ofFilter Paper - 47 mm Polycarbonate

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Filter (Approx 0.4 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 filter (approx 0.4 g) into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

374

Microwave Digestion ofFilter Paper - 47 mm Polycarbonate

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289

Microwave Digestion ofFilter Paper - Cellulose

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Filter (Approx 0.9 g)

ReagentsH₂OHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesAdd H₂O before HNO₃. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 filter (approx 0.9 g) of the sample into the digestion vessel. Add 5 mL of H₂O, and 5 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

372

Microwave Digestion ofFilter Paper - Cellulose

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290

Microwave Digestion ofGhost Wipe

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Wipe (Approx 2.5 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesEnsure that the entire wipe is covered with reagent.

ProcedureWeigh 1 wipe (approx 2.5 g) into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

375

Microwave Digestion ofGhost Wipe

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291

Microwave Digestion ofPaint Chips (For Pb Analysis)

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesHF may be required for a total dissolution.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, with some remaining inorganic particles upon dilution to 50 mL.

399

Microwave Digestion ofPaint Chips (For Pb Analysis)

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292

Microwave Digestion ofQuartz Fiber Filters

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.35 g (1 filter)

ReagentsHNO₃HF

Recommended VesselsMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis method should not exceed 180 degrees celsius.

This application should only be completed using the 75 mL Xpress or 110 mL Xpress Plus vessels. It is not suitable for the smaller Xpress vessels (55 mL, 20 mL, or 10 mL).

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureWeigh 1 filter (approximately 0.35 g) of the sample into the digestion vessel. Add 8 mL of HNO₃ and 2 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 20:00 15:00 N/A 1030-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSamples were clear, colorless, and particle free upon dilution to 50 mL with deionized water.

727

Microwave Digestion ofQuartz Fiber Filters

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293

Microwave Digestion ofToray Filter

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Filter (Approx 0.3 - 0.5 g)

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 1 filter (approximately 0.3-0.5 g) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 20:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

376

Microwave Digestion ofToray Filter in iPrep

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294

Microwave Digestion ofToray Filter (Anion)

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Filter (Approx 0.3 - 0.5 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureAdd 1 toray filter (Approx. 0.3 - 0.5 g) into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

561

Microwave Digestion ofToray Filter (Anion)

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295

Microwave Digestion ofToray Filter (Cation)

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Filter (Approx 0.3 -0.5 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureAdd 1 toray filter (Approx. 0.3 - 0.5 g) into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 20:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

562

Microwave Digestion ofToray Filter (Cation)

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Materials Science

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297

Microwave Digestion ofAcrylic Tape

Materials MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃DI H₂OHClHF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 3 mL of Deionized water, 7 mL of HNO₃, 1.5 mL of HCl, and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 30:00 10:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

720

Microwave Digestion ofAcrylic Tape in iPrep

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298

Microwave Digestion ofBismuth Aluminate Mixture

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHClHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 9 mL HCl and 3 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 190 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon diltuion to 50 mL.

746

Microwave Digestion ofBismuth Aluminate Mixture

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299

Microwave Digestion ofBismuth Yttrium Iron Oxide

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeHCl

Heating Program

Max Sample Weight0.1 g

ReagentsHCLHNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

HF should be added slowly and carefully to the sample.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 6 mL of HCl, 2 mL of HNO₃, and 0.5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 25:00 15:00 N/A 700-1800 Off

Microwave Digestion ofBismuth Yttrium Iron Oxide in iPrep (Step 1 of 2)

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300

Microwave Digestion ofBismuth Yttrium Iron Oxide

GeoscienMARS 6 (

ProcedureAllow vessel to cool. Add 1.75 g of solid H₃BO₃ + 20 mL deionized H₂O into the vessel that contains the sample and acid.

ReagentsSolid H₃BO₃DI H₂O

NotesThis procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction of certain analytes with hydrofluoric acid.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeStandard

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 25:00 10:00 N/A 700-1800 Off

General Precautiona) If using HF, follow restrictions listed in HF Addendum.b) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, yellow in color, and particle free upon dilution to 50 mL.

743

Microwave Digestion ofBismuth Yttrium Iron Oxide in iPrep (Step 2 of 2)

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301

Microwave Digestion ofCeramic Powder

Materials MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HFBoric Acid (solid)H₂O

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. It is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed with boric acid.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 5 mL of HNO₃, 10 mL of HF, 4.4 g of Boric Acid solid, and 25 mL of H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 195 15:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

752

Microwave Digestion ofCeramic Powder

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302

Microwave Digestion ofCeramic Powder

Materials MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HFBoric Acid (solid)H₂O

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis Application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed with boric acid.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 5 mL of HNO₃, 10 mL of HF, 4.4 g of Boric Acid solid, and 25 mL of H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 195 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

753

Microwave Digestion ofCeramic Powder in iPrep

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303

Microwave Digestion ofCircuit Board (Cryo - Ground)

Materials MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHClHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesHCl should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel. This method is considered a leach and may not provide a total digestion.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 3 mL of HNO₃ and 9 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 1030-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, with particles upon dilution to 50 mL.

377

Microwave Digestion ofCircuit Board (Cryo - Ground)

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304

Microwave Digestion ofFerric Oxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHClHNO₃DI H₂O

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 10 mL of a 1:1:1 HCl, HNO₃, and Deionized H₂O mixture. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 25:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, yellow in color, and particle free upon dilution to 50 mL.

744

Microwave Digestion ofFerric Oxide in iPrep

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305

Microwave Digestion ofGadolinium Zirconium Oxide

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeStandard

Heating Program

Max Sample Weight0.1 g

ReagentsH₂SO₄HNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

HF should be added slowly and carefully to the sample.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 4 mL of H₂SO₄, 1.5 mL of HNO₃ and 1.5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 280 35:00 30:00 N/A 700-1800 High

Microwave Digestion ofGadolinium Zirconium Oxide in iPrep (Step 1 of 2)

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306

Microwave Digestion ofGadolinium Zirconium Oxide

GeoscienMARS 6 (

ProcedureAllow vessel to cool. Add 1.5 g of solid H₃BO₃ + 20 mL deionized H₂O into the vessel that contains the sample and acid.

ReagentsH₃BO₃DI H₂O

NotesThis procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction of certain analytes with hydrofluoric acid.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeStandard

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 25:00 10:00 N/A 700-1800 High

General Precautiona) If using HF, follow restrictions listed in HF Addendum.b) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

742

Microwave Digestion ofGadolinium Zirconium Oxide in iPrep (Step 2 of 2)

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307

Microwave Digestion ofGas Atomized Powder

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HClHF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 8 mL of HNO₃, 2 mL of HCl, and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSamples were clear, green in color and particle free upon dilution to 50 mL.

721

Microwave Digestion ofGas Atomized Powder in iPrep

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308

Microwave Digestion ofGlass (Ground)

Materials MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHClHFHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 2 mL of HNO₃, 4 mL of HCl, and 3 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

378

Microwave Digestion ofGlass (Ground)

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309

Microwave Digestion ofGraphite Composite - Cyanate Ester Resin

Materials MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1.5 g of the sample into the digestion vessel. Add 30 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 150 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

563

Microwave Digestion ofGraphite Composite - Cyanate Ester Resin

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310

Microwave Digestion ofGraphite Composite - Epoxy Resin

Materials MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1.0 g of the sample into the digestion vessel. Add 30 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 150 10:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

564

Microwave Digestion ofGraphite Composite - Epoxy Resin

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311

Microwave Digestion ofGraphite Composite - PEEK Resin

Materials MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1.0 g of the sample into the digestion vessel. Add 30 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 160 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

565

Microwave Digestion ofGraphite Composite - PEEK Resin

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312

Microwave Digestion ofGraphite Fiber - Cyanate Siloxane Resin

Materials MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Laminate Square (Approx. 1 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesSample must be completely covered with acid prior to digestion.

After digestion the samples are filtered and the fibers are rinsed with deionized water.

This method is for the gravimetric (weight) determination of fiber content.

ProcedureAdd 1 Laminate Square (Approx. 1 g) of the sample into the digestion vessel. Add 35 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 150 10:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was digested, but the fiber filler material is left undigested for subsequent gravimetric analysis.

567

Microwave Digestion ofGraphite Fiber - Cyanate Siloxane Resin

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313

Microwave Digestion ofGraphite Fiber - Epoxy Resin (Fiber Content)

Materials MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesSample must be completely covered with acid prior to digestion.

After digestion the samples are filtered and the graphite fibers are rinsed with deionized water.

This method is for the gravimetric (weight) determination of fiber content.

ProcedureWeigh 1 g of the sample into the digestion vessel. Add 30 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 150 10:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was digested, but the fiber filler material is left undigested for subsequent gravimetric analysis.

379

Microwave Digestion ofGraphite Fiber - Epoxy Resin (Fiber Content)

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314

Microwave Digestion ofPollucite Ore

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃ HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 3 mL of HNO₃ and 5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 25:00 25:00 N/A 700-1800 Off

Microwave Digestion ofPollucite Ore in iPrep (Step 1 of 2)

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315

Microwave Digestion ofPollucite Ore

GeoscienMARS 6 (

ProcedureAllow vessel to cool. Add 2.5 g H₃BO₃ and 25 mL of deionized H₂O into the vessel that contains the sample and acid.

ReagentsH₃BO₃ DI H₂O

NotesThis procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction of certain analytes with hydrofluoric acid.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 25:00 15:00 N/A 700-1800 Off

General Precautiona) If using HF, follow restrictions listed in HF Addendum.b) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.c) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and particle free upon dilution to 50 mL.

757

Microwave Digestion ofPollucite Ore in iPrep (Step 2 of 2)

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316

Microwave Digestion ofSiloxanes

Materials MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 2 mL of HNO₃ and 5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

760

Microwave Digestion ofSiloxanes

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Metals & Alloys

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318

Microwave Digestion ofAlpha - Alumina

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeHCl

Heating Program

Max Sample Weight0.5 g

ReagentsHCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The maximum number of vessels that can be run for this method is 6.

Ensure that particles are well suspended in acid mixture prior to sealing vessel.

Stirring may be helpful to keep particles suspended in solution during digestion.

ProcedureWeigh 0.5 g of sample into the digestion vessel. Add 10 mL HCl. Gently swirl the vessel to thoroughly mix the sample and acid.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 59:59 N/A 900-1800 N/A

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

343

Microwave Digestion ofAlpha - Alumina in iPrep

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319

Microwave Digestion ofAluminum (Metal)

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHCl DI H₂O

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesHCl should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HCl and 3 mL of DI H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

382

Microwave Digestion ofAluminum (Metal)

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320

Microwave Digestion ofAluminum Alloy

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHClH₂O

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesAdd H₂O before HCl. Add HCl slowly, and allow vessels to stand in the fume hood until initial reaction subsides.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 5 mL of H₂O and 5 mL of HCl .Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 190 10:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

381

Microwave Digestion ofAluminum Alloy

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321

Microwave Digestion ofAluminum Alloy (20% SiC)

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization". The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 5 mL of HCl and 5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

569

Microwave Digestion ofAluminum Alloy (20% SiC)

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322

Microwave Digestion ofAluminum Alloy (BCS 182)

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHClH₂O₂ (30%)HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization". The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 20 mL of HCl, 10 mL of H₂O₂ (30%), and 5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 10:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

568

Microwave Digestion ofAluminum Alloy (BCS 182)

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323

Microwave Digestion ofAluminum Oxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsH₃PO₄H₂SO₄

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesEasyPrep Plus requires a high temperature probe for this method.

Ensure that particles are well suspended in acid mixture prior to sealing vessel.

Stirring may be helpful to keep particles suspended in solution during digestion.

ProcedureWeigh 0.25 g of sample into the digestion vessel. Add 6.5 mL H₃PO₄ and 3.5 mL H₂SO₄. Gently swirl the vessel to thoroughly mix the sample and acid.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 270 30:00 20:00 N/A 900-1800 N/A

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

344

Microwave Digestion ofAluminum Oxide

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324

Microwave Digestion ofAluminum Oxide (H₃PO₄)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1g

ReagentsH₃PO₄

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This method may not provide a total digest of all samples. Hydrofluoric acid may be required to provide complete digestion of some sample matrixes.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 8 mL H₃PO₄. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 260 25:00 45:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and colorless with some white particles remaining upon dilution to 50 mL.

673

Microwave Digestion ofAluminum Oxide (H3PO4) in iPrep

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325

Microwave Digestion ofBoron

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 5 mL of HNO₃ and 5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 175 15:00 25:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

570

Microwave Digestion ofBoron

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326

Microwave Digestion ofBoron Carbide (B₄C)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃H₂SO₄HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “BoricAcid HF Neutralization”.

Reducing the particle size increases the efficiency of digestion and may decrease the digestion time.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 5 mL of HNO₃ and 5 mL of H₂SO₄. Gently swirl to mix the sample particles in the acid. Slowly and carefully add 5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 270 30:00 30:00 800 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

674

Microwave Digestion ofBoron Carbide (B4C) in iPrep

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327

Microwave Digestion ofCarbonyl Iron

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HClHBF₄

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 6 mL HNO₃, 2 mL HCl, and 1 mL HBF₄ slowly. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, yellow in color with no visible particles upon dilution to 50 mL.

678

Microwave Digestion ofCarbonyl Iron in iPrep

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328

Microwave Digestion ofCobalt - Chromium Alloy (Co-Cr)

Metals anMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HFDI H₂O

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization". Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

ProcedureAdd 0.5 g of the sample into the digestion vessel. Add 5 mL of HNO₃, 5 mL of HF, and 5 mL of deionized H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

Microwave Digestion ofCobalt - Chromium Alloy (Co-Cr) (Step 1 of 2)

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329

Microwave Digestion ofCobalt - Chromium Alloy (Co-Cr)

Metals anMARS 6 (

ProcedureAllow vessels to cool. Open and add 4 mL of H₂O₂ (30%) dropwise. Wait approximately 15 minutes before closing the vessel.

ReagentsH₂O₂ (30%)

Notes

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

572

Microwave Digestion ofCobalt - Chromium Alloy (Co-Cr) (Step 2 of 2)

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330

Microwave Digestion ofCopper (Metal)

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

384

Microwave Digestion ofCopper (Metal)

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331

Microwave Digestion ofCopper Ore

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃, HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis method is intended to be an acid leach, not a total digest. Hydrofluoric acid will be required to provide complete digestion of the sample matrix. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 mL of Aqua Regia (3:1 HCl:HNO₃ ,). Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, and colorless with some remaining particles upon dilution to 50 mL.

383

Microwave Digestion ofCopper Ore

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332

Microwave Digestion ofGallium

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsHNO₃ HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 2 mL of HNO₃ and 8 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

573

Microwave Digestion ofGallium

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333

Microwave Digestion ofIron - Chromium Alloy

Metals anMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHClHFDI H₂O

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization". The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureAdd 0.5 g of the sample into the digestion vessel. Add 5 mL of HCl, 5 mL of HF, and 2 mL of deionized H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

Microwave Digestion ofIron - Chromium Alloy (Step 1 of 2)

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334

Microwave Digestion ofIron - Chromium Alloy

Metals anMARS 6 (

ProcedureAllow vessels to cool. Open and add 5 mL of HNO₃. Wait approximately 15 minutes before closing the vessel.

ReagentsHNO₃

Notes

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

575

Microwave Digestion ofIron - Chromium Alloy (Step 2 of 2)

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335

Microwave Digestion ofIron - Chromium Alloy

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHClHFHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 5 mL of HCl, 5 mL of HF, and 5 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 30:00 15:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

685

Microwave Digestion ofIron - Chromium Alloy in iPrep

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336

Microwave Digestion ofIron - Lignosulfonate

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

574

Microwave Digestion ofIron - Lignosulfonate

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337

Microwave Digestion ofIron - Manganese Alloy

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization". The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HCl and 2 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

576

Microwave Digestion ofIron - Manganese Alloy

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338

Microwave Digestion ofIron - Silicon Alloy

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HFHCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Noteshis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HF, 5 mL HCl, and 3 mL HNO₃. Gently swirl the mixture and allow any initial reaction to subside before sealing vessel. HF should be added slowly and carefully to the sample.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

577

Microwave Digestion ofIron - Silicon Alloy

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339

Microwave Digestion ofLead Sulfide (PbS)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 5 mL of HNO₃ and 5 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

503

Microwave Digestion ofLead Sulfide (PbS)

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340

Microwave Digestion ofLithium Nickel Cobalt Manganese Oxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HCl

Recommended VesselsMARSXpress

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 4 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 10:00 N/A 1030-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsThe samples were clear, green in color, and particle free upon dilution.

724

Microwave Digestion ofLithium Nickel Cobalt Manganese Oxide

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341

Microwave Digestion ofMagnesium Oxide (MgO 40 -54 %)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsH₂O (deionized)HClHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution.The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 5 mL of DI H₂O, 5 mL HCl, and 5 mL HNO₃. Gently swirl and allow approximately 15 minutes for pre-digestion.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

762

Microwave Digestion ofMagnesium Oxide (MgO 40-54%)

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342

Microwave Digestion ofManganous Oxide (MnO)

GeoscienMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.2g of the sample into the digestion vessel. Add 10 mL HNO₃ and 3 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 10:00 800 900-1800 Off

Microwave Digestion ofManganous Oxide (MnO) (Step 1 of 2)

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343

Microwave Digestion ofManganous Oxide (MnO)

GeoscienMARS 6 (

ProcedureAllow vessel to cool after completion of Step 1. Open and add 5 mL of HCl. Gently swirl the mixture and seal the vessel.

ReagentsHCl

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

505

Microwave Digestion ofManganous Oxide (MnO) (Step 2 of 2)

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344

Microwave Digestion ofMetal Alloy - FeCr

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHClHFHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization”

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 5 mL of HCl, 5 mL of HNO₃, and 5 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

385

Microwave Digestion ofMetal Alloy - FeCr

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345

Microwave Digestion ofMetal Alloy - NiCr

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsH₂OHNO₃ HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization”

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 5 mL of H₂O, 5 mL of HNO₃, and 5 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

386

Microwave Digestion ofMetal Alloy - NiCr

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346

Microwave Digestion ofMetal Alloy (Ag, Au, Cu)

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeHCl

Heating Program

Max Sample Weight0.1 g

ReagentsHClHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This method may not provide a total digest of all samples. Hydrofluoric acid may be required to provide complete digestion of some sample matrices.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 9 mL HCl, 1 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 25:00 25:00 N/A 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was yellow in color, with some white particles remaining upon dilution to 50 mL.

686

Microwave Digestion ofMetal Alloy (Ag, Au, Cu) in iPrep

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347

Microwave Digestion ofMetal Alloy (Ag, Co, Cu)

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃Deionized H₂OHF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 3 mL HNO₃, 3 mL Deionized H₂O and 3 mL HF (in this order). Add HF slowly and carefully. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 25:00 25:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

687

Microwave Digestion ofMetal Alloy (Ag, Co, Cu) in iPrep

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348

Microwave Digestion ofMetal Alloy (Ag, Cu, Sn)

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃DI H₂OHF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 3 mL HNO₃, 3 mL Deionized Water, and 3 mL HF in this order. Add HF slowly and carefully. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 25:00 25:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

688

Microwave Digestion ofMetal Alloy (Ag, Cu, Sn) in iPrep

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349

Microwave Digestion ofMetal Ore - Precious

Metals anMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃ HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization”

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 10 mL of HNO₃, and 0.5 ml of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 20:00 800 900-1800 Off

Microwave Digestion ofMetal Ore - Precious (Step 1 of 2)

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350

Microwave Digestion ofMetal Ore - Precious

Metals anMARS 6 (

ProcedureCool, vent and open vessel after step 1. Add 5 ml of HCl.

ReagentsHCl

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 10:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

603

Microwave Digestion ofMetal Ore - Precious (Step 2 of 2)

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351

Microwave Digestion ofMetals Alloy (Co-Cr)

Metals anMARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HFH2O

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Deionized Water may improve solubility of metal alloys.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 5 ml of HNO₃, 5 ml of HF, and 5 of ml H2O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

Microwave Digestion ofMetals Alloy (Co-Cr) (Step 1 of 2)

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352

Microwave Digestion ofMetals Alloy (Co-Cr)

Metals anMARS 6 (

ProcedureCool, vent and open vessel after step 1. Add 4 ml of H₂O₂, (30%)

ReagentsH₂O₂

Notes

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 10:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

602

Microwave Digestion ofMetals Alloy (Co-Cr) (Step 2 of 2)

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353

Microwave Digestion ofNickel (II) Hydroxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HCl

Recommended VesselsMARSXpress

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 4 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 10:00 N/A 1030-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsThe samples were clear, light green in color, and particle free upon dilution.

725

Microwave Digestion ofNickel (II) Hydroxide

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354

Microwave Digestion ofNickel (Metal)

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃DI H₂O

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of sample into the digestion vessel. Add 5 mL of HNO₃ and 5 mL of DI H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

387

Microwave Digestion ofNickel (Metal)

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355

Microwave Digestion ofNiobium - Titanium Alloy

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHFHNO₃DI H₂O

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Noteshis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 1 mL of HF, 5 mL HNO₃, and 5 mL of deionized H₂O. Gently swirl the mixture and wait approximately 15 minutes before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

578

Microwave Digestion ofNiobium - Titanium Alloy

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356

Microwave Digestion ofPhosphate (21%)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsH₂O₂ (30%)HClHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 5 mL of H₂O₂ (30%), 5 mL HCl dropwise (wait for reaction to subside before adding next acid), and 5 mL HNO₃. Gently swirl the mixture and wait approximately 1 hour before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

761

Microwave Digestion ofPhosphate (21%)

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357

Microwave Digestion ofPlatinum Metal

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of Aqua Regia (3:1 HCl:HNO₃). Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

388

Microwave Digestion ofPlatinum Metal

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358

Microwave Digestion ofPlatinum Ruthenium

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeHCl

Heating Program

Max Sample Weight0.1 g

ReagentsHClHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 6 mL of HCl, and 2 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 59:59 N/A 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

694

Microwave Digestion ofPlatinum Ruthenium in iPrep

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359

Microwave Digestion ofRhodium Sponge

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeHCl

Heating Program

Max Sample Weight0.1 g

ReagentsHClH₂O₂

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The maximum number of vessels that can be run with this method is 6.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 10 mL of HCl and 2 mL of H₂O₂ dropwise. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 250 25:00 45:00 N/A 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and colorless upon dilution to 50 mL.

697

Microwave Digestion ofRhodium Sponge in iPrep

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360

Microwave Digestion ofSelenium Alloy

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1 g (0.5 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

389

Microwave Digestion ofSelenium Alloy

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361

Microwave Digestion ofSn - Ag Solder

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsH₂OHNO₃HF

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesCaution must be taken when adding the acid solution to the sample as the reaction is very vigorous and exothermic.

Allow any initial reaction to subside before sealing the vessel.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Slowly add dropwise 10 ml of 1:1:1 H₂O:HNO₃:HF (premixed) to the sample. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

390

Microwave Digestion ofSn - Ag Solder

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362

Microwave Digestion ofStainless and Low Carbon Steel

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeHCl

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureAdd 0.25 g of the sample into the digestion vessel. Add 3 mL of HNO₃, and 9 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 25:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, gold colored, and particle free upon dilution to 50 mL.

704

Microwave Digestion ofStainless and Low Carbon Steel in iPrep

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363

Microwave Digestion ofStainless Steel

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HFHCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization”

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 ml of HCl, 3 mL of HNO₃, and 3 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

391

Microwave Digestion ofStainless Steel

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364

Microwave Digestion ofSteel (Stainless)

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHClHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis method may not provide a total digest of all samples. Hydrofluoric acid will be required to provide complete digestion of some sample matrixes.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 3 mL of HNO₃ and 9 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

392

Microwave Digestion ofSteel (Stainless)

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365

Microwave Digestion ofStrontium Ferrite

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeHCl

Heating Program

Max Sample Weight0.5 g

ReagentsHClHF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution.

ProcedureWeigh 0.5 g of sample into the digestion vessel. Add 10 mL of HCl and 0.5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 30:00 15:00 N/A 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

705

Microwave Digestion ofStrontium Ferrite in iPrep

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366

Microwave Digestion ofTitanium Alloy

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HFHCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric HF Neutralization”

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 5 mL of HNO₃, 2 mL of HCl, and 5 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

479

Microwave Digestion ofTitanium Alloy

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367

Microwave Digestion ofTitanium Dioxide

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃ and 2 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

489

Microwave Digestion ofTitanium Dioxide

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368

Microwave Digestion ofTungsten Ore (50% W; 10% Fe; 2% Mn)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHClHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 9 mL of HCl and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 25:00 20:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

513

Microwave Digestion ofTungsten Ore (50% W; 10% Fe; 2% Mn)

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369

Microwave Digestion ofZinc Oxide (ZnO)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 5 mL of HNO₃ and 2 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

393

Microwave Digestion ofZinc Oxide (ZnO)

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370

Microwave Digestion ofZinc Oxide (ZnO)

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.25 g of the sample (onto a filter disk) into the digestion vessel. Add 5 mL HNO₃ and 2 mL HF. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 25:00 15:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

712

Microwave Digestion ofZinc Oxide (ZnO) in iPrep

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371

Microwave Digestion ofZircon Alloy

Metals anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHFHNO₃DI H₂O

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureAdd 1.0 g of the sample into the digestion vessel. Add 5 mL of HF, 1 mL HNO₃, and 10 mL of deionized H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

580

Microwave Digestion ofZircon Alloy

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Nutraceuticals

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373

Nutraceuticals

Microwave Digestion ofBiotin

NutraceutiMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

394

Microwave Digestion ofBiotin

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374

Microwave Digestion ofCannabis (Plant)

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃, or alternatively 9 mL HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

715

Microwave Digestion ofCannabis (Plant)

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375

Microwave Digestion ofChili Powder

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2 g

ReagentsHNO₃DI H₂O

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 2 g of the sample into the digestion vessel. Add 10 mL HNO₃ and 5 mL deionized H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and colorless with some small particles (silicates) remaining upon dilution to 50 mL.

680

Microwave Digestion ofChili Powder in iPrep

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376

Microwave Digestion ofCitrus Leaves

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃DI H₂OHF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 6 mL of HNO₃, 3 mL of deionized H₂O, and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

539

Microwave Digestion ofCitrus Leaves

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377

Microwave Digestion ofGinkgo (Ground)

NutraceutiMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

395

Microwave Digestion ofGinkgo (Ground)

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378

Microwave Digestion ofGinkgo (Whole Pill)

NutraceutiMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Pill (Approx 1.0 g)

ReagentsHNO₃H₂O₂

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 pill (approx 1.0 g) into the digestion vessel. Add 10 mL of HNO₃ and 2 mL of H₂O₂. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

396

Microwave Digestion ofGinkgo (Whole Pill)

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379

Microwave Digestion ofInfant Formula (Liquid)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight2 mL

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 2 mL of of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Results Sample was clear, colorless and particle free upon dilution to 50 mL

301

Microwave Digestion ofInfant Formula (Liquid) in iPrep

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380

Microwave Digestion ofInfant Formula (Liquid)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 1 mL (0.5 mL w/Xpress Vessels) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

302

Microwave Digestion ofInfant Formula (Liquid)

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381

Microwave Digestion ofInfant Formula (Powder)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

303

Microwave Digestion ofInfant Formula (Powder) in iPrep

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382

Microwave Digestion ofInfant Formula (Powder)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

304

Microwave Digestion ofInfant Formula (Powder)

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383

Microwave Digestion ofKelp

NutraceutiMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight 0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

421

Microwave Digestion ofKelp

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384

Microwave Digestion ofMilk (Whole - Liquid)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight4 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 4 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

309

Microwave Digestion ofMilk (Whole - Liquid)

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385

Microwave Digestion ofMilk (Powder)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

310

Microwave Digestion ofMilk (Powder)

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386

Microwave Digestion ofPlant Tissue

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis. Some plant tissues contain silicates which would require HF for total dissolution.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

234

Microwave Digestion ofPlant Tissue

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387

Microwave Digestion ofUSP 232/233 (Pharmaceuticals)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL HCl. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

265

Microwave Digestion ofUSP 232/233 (Pharmaceuticals)

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388

Microwave Digestion ofWheat

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

239

Microwave Digestion ofWheat

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389

Microwave Digestion ofWhey (Powder)

Food TestMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

339

Microwave Digestion ofWhey (Powder)

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Organic Chemicals

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391

Microwave Digestion ofDi-(2-ethylhexyl)phosphoric Acid

Organic CMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 mL

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureTransfer 0.5 mL of the sample into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 30:00 15:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

682

Microwave Digestion ofDi-(2-ethylhexyl)phosphoric Acid in iPrep

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392

Microwave Digestion ofDiazo Sulfonyl Chloride

Organic CMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

581

Microwave Digestion ofDiazo Sulfonyl Chloride

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393

Microwave Digestion ofFood Coloring (Erythrosine Based)

Organic CMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

582

Microwave Digestion ofFood Coloring (Erythrosine Based)

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394

Microwave Digestion ofMethylcellulose (Hydroxypropyl)

Organic CMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃DI H₂O

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 10 mL of HNO₃ and 2 mL of deionized H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

583

Microwave Digestion ofMethylcellulose (Hydroxypropyl)

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395

Microwave Digestion ofMonoethanolamine

Organic CMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 5 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

584

Microwave Digestion ofMonoethanolamine

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396

Microwave Digestion ofPhotoresist

Organic CMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureAdd 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

398

Microwave Digestion ofPhotoresist

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397

Microwave Digestion ofPolygluteramide

Organic CMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

585

Microwave Digestion ofPolygluteramide

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Paints & Coatings

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399

Microwave Digestion ofPaint (Latex Based Liquid)

Paints anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesHF is required for a total dissolution of inorganic filler if present.

If this procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 1 g (0.5 g w/Xpress Vessels) of sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

400

Microwave Digestion ofPaint (Latex Based Liquid)

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400

Microwave Digestion ofPaint Chips (For Pb Analysis)

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesHF may be required for a total dissolution.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, with some remaining inorganic particles upon dilution to 50 mL.

399

Microwave Digestion ofPaint Chips (For Pb Analysis)

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401

Microwave Digestion ofPhotoresist

Organic CMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureAdd 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

398

Microwave Digestion ofPhotoresist

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402

Microwave Digestion ofPolyurethane

Paints anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

468

Microwave Digestion ofPolyurethane

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403

Microwave Digestion ofPolyurethane

Paints anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 6 mL HNO₃, and 3 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

696

Microwave Digestion ofPolyurethane in iPrep

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404

Microwave Digestion ofToner (Ink)

Paints anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel. The use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 20:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless with some particles remaining upon dilution to 50 mL.

401

Microwave Digestion ofToner (Ink) in iPrep

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405

Microwave Digestion ofToner (Powder)

Paints anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The use of HF may be required to digest any silicates found in the sample.

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.e) If using HF, follow restrictions listed in HF Addendum.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

709

Microwave Digestion ofToner (Powder) in iPrep

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Paper & Pulp

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407

Microwave Digestion ofFilter Paper - 37 mm Mixed Cellulose Ester

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Filter (Approx 0.3 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 filter (approx 0.3 g) into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

373

Microwave Digestion ofFilter Paper - 37 mm Mixed Cellulose Ester

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408

Microwave Digestion ofFilter Paper - 47 mm Polycarbonate

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Filter (Approx 0.4 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 filter (approx 0.4 g) into the digestion vessel. Add 10 mL HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

374

Microwave Digestion ofFilter Paper - 47 mm Polycarbonate

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409

Microwave Digestion ofFilter Paper - Cellulose

Industrial MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Filter (Approx 0.9 g)

ReagentsH₂OHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesAdd H₂O before HNO₃. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 filter (approx 0.9 g) of the sample into the digestion vessel. Add 5 mL of H₂O, and 5 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

372

Microwave Digestion ofFilter Paper - Cellulose

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410

Microwave Digestion ofPaper Pulp

Paper anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

473

Microwave Digestion ofPaper Pulp

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Personal Care

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412

Microwave Digestion ofBoric Acid HF Neutralization

AgriculturMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample WeightVaries by Sample

ReagentsH₃BO₃ (4%)

Recommended VesselsEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction of certain analytes with hydrofluoric acid.

Alternatively, 1-4 g of solid H₃BO₃ + 25 mL deionized H₂O can be used in place of the 4% w/v solution.

ProcedureAllow vessel to cool. Add 30 mL H₃BO₃ (4%) into the vessel that contains the sample and acid.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSee sample specific method notes.

6

Microwave Digestion ofBoric Acid HF Neutralization

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413

Microwave Digestion ofCosmetics (Liquid Make-Up)

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 8 mL of HNO₃ and 2 mL of HF. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

246

Microwave Digestion ofCosmetics (Liquid Make-Up)

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414

Microwave Digestion ofEye Shadow

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 7 mL of HNO₃ and 3 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL

247

Microwave Digestion ofEye Shadow

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415

Microwave Digestion ofShampoo (Dandruff)

ConsumeMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 mL

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe use of HF may be required to digest any silicates found in the sample.

ProcedureTransfer 1 mL of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

248

Microwave Digestion ofShampoo (Dandruff)

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Pharmaceutical & Biotech

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417

Microwave Digestion ofAllergy Pill (Ground)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain therequired results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at orbelow room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vesselsdetected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

402

Microwave Digestion ofAllergy Pill (Ground)

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418

Microwave Digestion ofAllergy Pill (Whole Pill)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Pill (Approx 1.0 g)

ReagentsHNO₃H₂O₂ (30%)

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 pill (Approx 1.0 g) into the digestion vessel. Add 10 mL of HNO₃ and 2 mL of H₂O₂ (30%). Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

403

Microwave Digestion ofAllergy Pill (Whole Pill)

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419

Microwave Digestion ofAntioxidant (Ground)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

404

Microwave Digestion ofAntioxidant (Ground)

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420

Microwave Digestion ofAntioxidant (Whole Pill)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Pill (Approx 1.4 g)

ReagentsHNO₃H₂O₂ (30%)

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 pill (approx 1.4 g) into the digestion vessel. Add 10 mL of HNO₃ and 2 mL of H₂O₂ (30%). Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

405

Microwave Digestion ofAntioxidant (Whole Pill)

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421

Microwave Digestion ofAPIs with Aromatic Ring Structures

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 250 30:00 25:00 N/A 700-1800 N/A

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL. If the sample contains precious metals the diluted sample may be the color associated with the metals.

406

Microwave Digestion ofAPIs with Aromatic Ring Structures in iPrep

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422

Microwave Digestion ofAscorbic Acid

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

407

Microwave Digestion ofAscorbic Acid

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423

Microwave Digestion ofAspirin (Ground)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

408

Microwave Digestion ofAspirin (Ground)

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424

Microwave Digestion ofAspirin (Whole)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight 1 pill (Approx 1.0 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 pill (Approx 1.0 g) into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

409

Microwave Digestion ofAspirin (Whole)

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425

Microwave Digestion ofBeta Carotene

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

410

Microwave Digestion ofBeta Carotene

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426

Microwave Digestion ofBiotin

NutraceutiMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

394

Microwave Digestion ofBiotin

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427

Microwave Digestion ofCalcium Carbonate

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis. Allow initial reaction to subside before sealing vessel.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Slowly add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

411

Microwave Digestion ofCalcium Carbonate

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428

Microwave Digestion ofCalpan Pantothenic Acid

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight 0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

412

Microwave Digestion ofCalpan Pantothenic Acid

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429

Microwave Digestion ofCephalexin

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

413

Microwave Digestion ofCephalexin

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430

Microwave Digestion ofChromium Chelate

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Resultsample was clear, colorless, and particle free upon dilution to 50 mL.

414

Microwave Digestion ofChromium Chelate

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431

Microwave Digestion ofCold and Flu Medicine (Liquid)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.75 mL

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 0.75 mL of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

415

Microwave Digestion ofCold & Flu Medicine (Liquid)

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432

Microwave Digestion ofCupric Sulfate

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, blue in color, and particle free upon dilution to 50 mL.

416

Microwave Digestion ofCupric Sulfate

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433

Microwave Digestion ofDiclofenac K

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃H₂O₂ (30%)

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃ and 2 mL of H₂O₂ (30%). Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

417

Microwave Digestion ofDiclofenac K

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434

Microwave Digestion ofEmpty Capsule (Gel)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Capsule (Approx 0.1 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 capsule (Approx 0.1 g) into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

418

Microwave Digestion ofEmpty Capsule (Gel)

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435

Microwave Digestion ofErythromycin

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

586

Microwave Digestion ofErythromycin

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436

Microwave Digestion ofFish Oil (No Capsule)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

419

Microwave Digestion ofFish Oil (No Capsule)

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437

Microwave Digestion ofFlurbiprofen

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

587

Microwave Digestion ofFlurbiprofen

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438

Microwave Digestion ofFolic Acid

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

420

Microwave Digestion ofFolic Acid

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439

Microwave Digestion ofGinkgo (Ground)

NutraceutiMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

395

Microwave Digestion ofGinkgo (Ground)

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440

Microwave Digestion ofGinkgo (Whole Pill)

NutraceutiMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Pill (Approx 1.0 g)

ReagentsHNO₃H₂O₂

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 pill (approx 1.0 g) into the digestion vessel. Add 10 mL of HNO₃ and 2 mL of H₂O₂. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

396

Microwave Digestion ofGinkgo (Whole Pill)

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441

Microwave Digestion ofHydrocodone

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 25:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

588

Microwave Digestion ofHydrocodone

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442

Microwave Digestion ofIbuprofen (Ground)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”.

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 8 mL HNO₃ and 2 mL HF. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 20:00 15:00 800 1030-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

730

Microwave Digestion ofIbuprofen (Ground)

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443

Microwave Digestion ofKelp

NutraceutiMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight 0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

421

Microwave Digestion ofKelp

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444

Microwave Digestion ofLosartan K

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃H₂O₂ (30%)

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃ and 2 mL of H₂O₂ (30%). Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

422

Microwave Digestion ofLosartan K

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445

Microwave Digestion ofMagnesium Carbonate

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesAllow any reaction to subside before sealing the vessel. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

423

Microwave Digestion ofMagnesium Carbonate

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446

Microwave Digestion ofMagnesium Oxide

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

424

Microwave Digestion ofMagnesium Oxide

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447

Microwave Digestion ofManganese Carbonate

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

426

Microwave Digestion ofManganese Carbonate

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448

Microwave Digestion ofMedroxyprogesterone

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

589

Microwave Digestion ofMedroxyprogesterone

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449

Microwave Digestion ofMetformin (Ground)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

427

Microwave Digestion ofMetformin (Ground)

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450

Microwave Digestion ofMineral Oil

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

459

Microwave Digestion ofMineral Oil

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451

Microwave Digestion ofMultivitamin (Ground)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

428

Microwave Digestion ofMultivitamin (Ground)

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452

Microwave Digestion ofMultivitamin (Whole)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Pill (Approx 2.5 g)

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 pill (Approx 2.5 g) into the digestion vessel. Add 10 mL of HNO₃ and 2 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

429

Microwave Digestion ofMultivitamin (Whole)

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453

Microwave Digestion ofNaproxen Sodium

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃ and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 25:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

590

Microwave Digestion ofNaproxen Sodium

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454

Microwave Digestion ofNiacinamide

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight 0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

430

Microwave Digestion ofNiacinamide

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455

Microwave Digestion ofPantothenic Acid

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

431

Microwave Digestion ofPantothenic Acid

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456

Microwave Digestion ofPotassium Chelate

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

432

Microwave Digestion ofPotassium Chelate

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457

Microwave Digestion ofProtopic Ointment

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 25:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

591

Microwave Digestion ofProtopic Ointment

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458

Microwave Digestion ofPyridoxine

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight 0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended Equipment

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

434

Microwave Digestion ofPyridoxine

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459

Microwave Digestion ofRiboflavin

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 20:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

435

Microwave Digestion ofRiboflavin

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460

Microwave Digestion ofSelenium Chelate

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

436

Microwave Digestion ofSelenium Chelate

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461

Microwave Digestion ofSleep Aid

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃ and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 25:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

592

Microwave Digestion ofSleep Aid

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462

Microwave Digestion ofSodium Polystyrene Sulfonate

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsDI H₂OHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 6 mL of HNO₃ and 2 mL of deionized H₂O. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 250 25:00 25:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and colorless upon dilution to 50 mL.

703

Microwave Digestion ofSodium Polystyrene Sulfonate in iPrep

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463

Microwave Digestion ofStearic Acid

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

437

Microwave Digestion ofStearic Acid

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464

Microwave Digestion ofSudan Orange (4-Fluorophenyl)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃HCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 250 25:00 25:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

706

Microwave Digestion ofSudan Orange (4-Fluorophenyl) in iPrep

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465

Microwave Digestion ofThiamine

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight 0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

438

Microwave Digestion ofThiamine

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466

Microwave Digestion ofTransdermal Patch

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HClNH₄F

Recommended VesselsEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses ammonium fluoride, which creates in-situ hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 9 mL of HNO₃, 1 mL of HCl, and 0.1 g of NH₄F. Gently swirtl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsCompleted samples were clear, colorless and particle free upon dilution to 50 mL.

593

Microwave Digestion ofTransdermal Patch

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467

Microwave Digestion ofTrixie Phosphate

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight50 mg

ReagentsHNO₃HCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 50 mg of the sample into the digestion vessel. Add 6 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 250 30:00 25:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

710

Microwave Digestion ofTrixie Phosphate in iPrep

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468

Microwave Digestion ofUSP 232/233 (Pharmaceuticals)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL HCl. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

265

Microwave Digestion ofUSP 232/233 (Pharmaceuticals)

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469

Microwave Digestion ofVitamin B-12

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

439

Microwave Digestion ofVitamin B-12

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470

Microwave Digestion ofVitamin C (Ground)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

440

Microwave Digestion ofVitamin C (Ground)

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471

Microwave Digestion ofVitamin C (Whole)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Pill (Approx 1.4 g)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 1 pill (Approx 1.4 g) into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

441

Microwave Digestion ofVitamin C (Whole)

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472

Microwave Digestion ofVitamin Concentrate (High Fe)

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO3HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 5 mL of HNO3 and 5 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 180 15:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

519

Microwave Digestion ofVitamin Concentrate (High Fe)

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473

Microwave Digestion ofVitamin D

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 20:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

442

Microwave Digestion ofVitamin D

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474

Microwave Digestion ofVitamin D3

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

443

Microwave Digestion ofVitamin D3

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475

Microwave Digestion ofVitamin E

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃ HCl

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 9 mL of HNO₃, and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 20:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

444

Microwave Digestion ofVitamin E

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476

Microwave Digestion ofVitamins

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HFHCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric Acid HF Neutralization”. The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 9 mL of HNO₃, 1 mL HCl, and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

445

Microwave Digestion ofVitamins

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477

Microwave Digestion ofZinc Sulfate

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

446

Microwave Digestion ofZinc Sulfate

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Plastics, Polymers, & Oils

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479

Microwave Digestion ofAcrylamide

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

447

Microwave Digestion ofAcrylamide

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480

Microwave Digestion ofBrominated Flame Retardant

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeStandard

Heating Program

Max Sample Weight50 mg

ReagentsH₂SO₄HNO₃H₂O₂

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

Stirring is required for complete dissolution of this sample type.

ProcedureWeigh 50 mg of the sample into the digestion vessel. Insert stir bar into the vessel. Add 4.5 mL H₂SO₄ and 4.0 mL HNO₃ to the vessel, then add 1.5 mL H₂O₂ dropwise. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 270 30:00 45:00 N/A 900-1800 Med

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and colorless, and particle free upon dilution to 50 mL.

675

Microwave Digestion ofBrominated Flame Retardant in iPrep

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481

Microwave Digestion ofBunker Oil

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.3 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel. The pre-digestion step will allow the lighter fuel fractions to react before sealing the vessels.

ProcedureWeigh 0.3 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

451

Microwave Digestion ofBunker Oil in iPrep

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482

Microwave Digestion ofChar - Sulfuric Acid

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample WeightVaries by sample

ReagentsH₂SO₄

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesEasyPrep Plus requires a high temperature probe for this method. This method is for the pretreatment of large sample sizes or difficult organic samples that are resistant to oxidation. After the char is complete, the vessel is opened and a normal oxidation with HNO₃ can be run, usually at around 200C.

ProcedureAdd 6 mL H₂SO₄ into the vessel that contains the sample and acid.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 260 15:00 30:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSee sample specific method notes.

352

Microwave Digestion ofChar - Sulfuric Acid

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483

Microwave Digestion ofCrude Oil

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

452

Microwave Digestion ofCrude Oil

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484

Microwave Digestion ofDiesel Fuel

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe pre-digestion step will allow the lighter fuel fractions to react before sealing the vessels

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃ . Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

357

Microwave Digestion ofDiesel Fuel

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485

Microwave Digestion ofEpoxy Hardener

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

453

Microwave Digestion ofEpoxy Hardener

Page 486: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

486

Microwave Digestion ofFatty Alcohol

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃HCl

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.1 g of the sample into the digestion vessel. Add 2 mL of HNO₃ and 4 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

454

Microwave Digestion ofFatty Alcohol

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487

Microwave Digestion ofFluorinated Ethylene Propylene (FEP)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight120 mg

ReagentsH₂SO₄HNO₃H₂O₂

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 120 mg of the sample into the digestion vessel. Add 4.5 mL of H₂SO₄, 4 mL of HNO₃, and 1.5 mL of H₂O₂ slowly. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 280 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and colorless upon dilution to 50 mL.

717

Microwave Digestion ofFluorinated Ethylene Propylene (FEP) in iPrep

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488

Microwave Digestion ofFuel Oil (Slurry)

Plastics, MARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃ HF

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid or other neutralization step should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO₃ and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 250 30:00 30:00 N/A 700-1800 Off

Microwave Digestion ofFuel Oil (Slurry) in iPrep (Step 1 of 2)

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489

Microwave Digestion ofFuel Oil (Slurry)

Plastics, MARS 6 (

ProcedureAllow vessels to cool. Open and add 2 mL H₂O₂ (30%) dropwise. Wait approximately 15 minutes before closing the vessel.

ReagentsH₂O₂ (30%)

Notes

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear and colorless upon dilution to 50 mL.

650

Microwave Digestion ofFuel Oil (Slurry) in iPrep (Step 2 of 2)

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490

Microwave Digestion ofGasoline

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.1 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe pre-digestion step will allow the lighter fuel fractions to react before sealing the vessels.

ProcedureAdd 0.1 g of the sample into the digestion vessel. Slowly add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

455

Microwave Digestion ofGasoline

Page 491: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

491

Microwave Digestion ofGlycerol Ester of Wood Rosin (Ground)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.5 g (ground) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to predigest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL with deionized water.

684

Microwave Digestion ofGlycerol Ester of Wood Rosin (Ground) in iPrep

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492

Microwave Digestion ofHDPE

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

456

Microwave Digestion ofHDPE

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493

Microwave Digestion ofKerosene

GeoscienMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe pre-digestion step will allow the lighter fuel fractions to react before sealing the vessels.

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

359

Microwave Digestion ofKerosene

Page 494: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

494

Microwave Digestion ofKevlar

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel. Ensure that all fibers are completely covered with acid and not adhered to the vessel liner wall.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 250 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

457

Microwave Digestion ofKevlar in iPrep

Page 495: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

495

Microwave Digestion ofLube Oil

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

458

Microwave Digestion ofLube Oil

Page 496: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

496

Microwave Digestion ofMethyl Ester of Hydrogenated Wood Rosin (Ground)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃ . Gently swirl the mixture and wait approximately 15 minutes to predigest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL with deionized water.

689

Microwave Digestion ofMethyl Ester of Hydrogenated Wood Rosin (Ground) in iPrep

Page 497: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

497

Microwave Digestion ofMineral Oil

PharmaceMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

459

Microwave Digestion ofMineral Oil

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498

Microwave Digestion ofMotor Oil (New)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

460

Microwave Digestion ofMotor Oil (New)

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499

Microwave Digestion ofMotor Oil (Waste)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe pre-digestion step will allow the lighter fuel fractions to react before sealing the vessels.

ProcedureWeigh 0.25 g (0.1 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

360

Microwave Digestion ofMotor Oil (Waste)

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500

Microwave Digestion ofMotor Oil (Waste)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel. The pre-digestion step will allow the lighter fuel fractions to react before sealing the vessels.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 240 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

461

Microwave Digestion ofMotor Oil (Waste) in iPrep

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501

Microwave Digestion ofNylon

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

462

Microwave Digestion ofNylon

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502

Microwave Digestion ofOil Wear Metals

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

598

Microwave Digestion ofOil Wear Metals

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503

Microwave Digestion ofPET (Polyethylene Terephthalate)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃H₂SO₄

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 8 mL of HNO₃ and 2 mL of H₂SO₄. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

463

Microwave Digestion ofPET (Polyethylene Terephthalate)

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504

Microwave Digestion ofPET (Polyethylene Terephthalate)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.4 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.4 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 250 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

464

Microwave Digestion ofPET (Polyethylene Terephthalate) in iPrep

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505

Microwave Digestion ofPetrolatum

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

594

Microwave Digestion ofPetrolatum

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506

Microwave Digestion ofPlasticizer (Filter)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 6 mL HNO₃, and 3 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

691

Microwave Digestion ofPlasticizer (Filter) in iPrep

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507

Microwave Digestion ofPlasticizers

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution.The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 6 mL HNO₃ and 3 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

692

Microwave Digestion ofPlasticizers in iPrep

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508

Microwave Digestion ofPolycarbonate Resin

Plastics, MARS 6 (

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1.0 g

ReagentsH₂SO₄

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesEasy Prep Plus requires a high temperature probe for this method.

ProcedureChar Step Weigh 1.0 g of the sample into the digestion vessel. Add 6 mL of H₂SO₄. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 260 15:00 15:00 800 900-1800 Off

Microwave Digestion ofPolycarbonate Resin (Step 1 of 2)

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509

Microwave Digestion ofPolycarbonate Resin

Plastics, MARS 6 (

ProcedureProceeding step one, add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

ReagentsHNO₃

Notes

Heating Program

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL

604

Microwave Digestion ofPolycarbonate Resin (Step 2 of 2)

Page 510: Microwave Acid Digestion Method Note Compendium€¦ · Compendium October 1, 2019. Contents Agriculture Alfalfa 11 Boric Acid HF Neutralization 12 Cannabis (Plant) 13 Coffee Beans

510

Microwave Digestion ofPolyethersulfone (Filter Paper)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight1 Filter (Approx 0.1 g)

ReagentsHNO₃H₂SO₄

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 1 filter paper (Approx 0.1 g) into the digestion vessel. Add 8 mL of HNO₃ and 2 mL H₂SO₄. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

465

Microwave Digestion ofPolyethersulfone (Filter Paper)

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511

Microwave Digestion ofPolyethylene - High Density

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g (0.1 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 ml of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

466

Microwave Digestion ofPolyethylene - High Density

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512

Microwave Digestion ofPolyphenylene Sulfide

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

596

Microwave Digestion ofPolyphenylene Sulfide

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513

Microwave Digestion ofPolypropylene

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g (0.1 g w/Xpress)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 (0.1 g w/Xpress vessels) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

467

Microwave Digestion ofPolypropylene

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514

Microwave Digestion ofPolyterpene Resin

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in an iPrep.

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes to predigest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 30:00 30:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL with deionized water.

695

Microwave Digestion ofPolyterpene Resin in iPrep

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515

Microwave Digestion ofPolyurethane

Paints anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

468

Microwave Digestion ofPolyurethane

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516

Microwave Digestion ofPolyurethane

Paints anMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 6 mL HNO₃, and 3 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes to pre-digest before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless and particle free upon dilution to 50 mL.

696

Microwave Digestion ofPolyurethane in iPrep

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517

Microwave Digestion ofPVC (Polyvinyl Chloride Resin)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight 0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g (0.1 g w/Xpress Vessels) of sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

469

Microwave Digestion ofPVC (Polyvinyl Chloride Resin)

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518

Microwave Digestion ofRubber

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 220 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

471

Microwave Digestion ofRubber

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519

Microwave Digestion ofRubber (Synthetic)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 210 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

470

Microwave Digestion ofRubber (Synthetic)

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520

Microwave Digestion ofSilane Terminated Polyether

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HCl

Recommended VesselsiPrep

Recommended EquipmentMARS 6 iWave

NotesThis application can only be run in the iPrep vessel.

The addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes.

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 6 mL HNO₃ and 3 mL of HCl. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 30:00 20:00 N/A 700-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

699

Microwave Digestion ofSilane Terminated Polyether in iPrep

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521

Microwave Digestion ofSilicone Tubing - TiO₂ Filler

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃HF

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThis procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled "Boric Acid HF Neutralization".

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 2 mL HNO₃ and 5 mL of HF. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel. Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

557

Microwave Digestion ofSilicone Tubing - TiO2 Filler

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522

Microwave Digestion ofStyrene Acrylate

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

597

Microwave Digestion ofStyrene Acrylate

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523

Microwave Digestion ofTerephthalic Acid

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.2 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.2 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 230 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

472

Microwave Digestion ofTerephthalic Acid

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524

Microwave Digestion ofWax (Petroleum Based)

Plastics, MARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.25 g

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

595

Microwave Digestion ofWax (Petroleum Based)

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Water & Wastewater Treatment

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526

Microwave Digestion ofNPDES (Waste Water)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeWater

Heating Program

Max Sample Weight50 mL

ReagentsHNO₃ HCl

Recommended Vessels75 mL MARSXpressEasyPrepEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 50 mL of the sample into the digestion vessel. Add 3 mL of HNO₃, and 2 mL HCl. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 165 30:00 0:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

252

Microwave Digestion ofNPDES (Waste Water)

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527

Microwave Digestion ofSludge (Industrial)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe use of HF may be required to digest any silicates found in the sample. The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureWeigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO₃. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

257

Microwave Digestion ofSludge (Industrial)

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528

Microwave Digestion ofTCLP Extract

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeStandard Control

Sample TypeWater

Heating Program

Max Sample Weight25 mL

ReagentsHNO₃

Recommended VesselsEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 25 mL of the sample into the digestion vessel. Add 5 mL of HNO₃. Gently swirl the mixture before closing the vessel. If a high organic content is suspected, a 10 ml sample volume is recommended.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 10:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

259

Microwave Digestion ofTCLP Extract

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529

Microwave Digestion ofUS EPA 3015 (Aqueous Samples)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeStandard Control

Sample TypeWater

Heating Program

Max Sample Weight45 mL

ReagentsHNO₃

Recommended Vessels75 mL MARSXpressEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureTransfer 45 mL of the sample into the digestion vessel. Add 5 mL of HNO₃. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 10:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsThis method is intended to be an acid leach, not a total digest. Hydrofluoric acid will be required to provide complete digestion of the sample matrix.

260

Microwave Digestion ofUS EPA 3015 (Aqueous Samples)

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530

Microwave Digestion ofUS EPA 3015a (Aqueous Sample)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeStandard Control

Sample TypeWater

Heating Program

Max Sample Weight45 mL

ReagentsHNO₃HCl (Optional)

Recommended Vessels75 mL MARSXpressEasyPrep PlusMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

NotesThe addition of Conc. HCl (0-4 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. The amount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit the techniques or increase the difficulties of analysis.

ProcedureTransfer 45 mL of the sample into the digestion vessel. Add 5 mL of HNO3, or alternatively 4 mL of HNO₃ and 1 mL HCl. Gently swirl the mixture before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 10:00 10:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsThis method is intended to be an acid leach, not a total digest. Hydrofluoric acid will be required to provide complete digestion of the sample matrix.

261

Microwave Digestion ofUS EPA 3015a (Aqueous Sample)

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531

Microwave Digestion ofWaste Activated Sludge

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeOne Touch

Control TypeRamp to Temperature

Sample TypeOrganic

Heating Program

Max Sample Weight0.5 g (Dry Weight)

ReagentsHNO₃H₂O₂

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6MARS 6 iWave

Notes

ProcedureWeigh 0.5 g (dry weight) (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 5 mL of HNO₃, and 5 mL of H₂O₂. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 200 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

266

Microwave Digestion ofWaste Activated Sludge

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532

Microwave Digestion ofWater (For Analysis of Phosphorous)

EnvironmMARS 6

* Ramp times and power may vary depending on the type and number of vessels.

Method TypeClassic

Control TypeRamp to Temperature

Sample TypeWater

Heating Program

Max Sample Weight50 mL

ReagentsK₂S₂O₈ H₂SO₄

Recommended VesselsEasyPrepEasyPrep PlusMARSXpressMARSXpress Plus

Recommended EquipmentMARS 6

Notes

ProcedureTransfer 50 mL of H₂O into the digestion vessel. Add 0.5 g of K₂S₂O₈ and 1 mL of H₂SO₄. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

Stage Temp (°C) *Ramp (mm:ss) Hold (mm:ss) Pressure (psi) * Power (W) Stirring

1 170 15:00 15:00 800 900-1800 Off

General Precautiona) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

ResultsSample was clear, colorless, and particle free upon dilution to 50 mL.

267

Microwave Digestion ofWater (For Analysis of Phosphorous)