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i PREPARED BY: REVIEWED BY: APPROVED BY: c NAME n M/7$ flA/B&l IO// l9T 4 1% Ahrnad Ghandour Rich Dabolt Kelly McCurry v 4-402. DOCUMENT NO. PL-CNSI-98-004 1869 REV. 0 PAGE I OF 88 CHEM-NUCLEAR SYSTEMS INFORMATION ONLY 11 PRINTED OR TYPED 11 SIGNATURE 1 - DOCUMENT TITLE: U Fernald Proof of Principle Testing Project Work Plan

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Page 1: CHEM-NUCLEAR SYSTEMS - Department of Energy waste form properties (i.e., ... The following is a discussion of the chemical and physical ... indicate that only about 25% of the waste

i

PREPARED BY:

REVIEWED BY:

APPROVED BY:

c

NAME n

M / 7 $

flA/B&l I O / / l9T

4 1%

Ahrnad Ghandour

Rich Dabolt

Kelly McCurry

v

4-402.

DOCUMENT NO. PL-CNSI-98-004

1869

REV. 0 PAGE I OF 88

CHEM-NUCLEAR SYSTEMS INFORMATION ONLY

11 PRINTED OR TYPED 11 SIGNATURE 1-

DOCUMENT TITLE: U Fernald Proof of Principle Testing

Project Work Plan

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Table of Contents

1 . 0 INTRODUCTION ............................................................................................. 5

1.1 Project Description ............................................................................. 5 1.2 Test Objectives .................................................................................. 5

2.0 TREATMENT TECHNOLOGY DESCRIPTION ............................................... 6

2.1 Arsenic .................................................. : ............................................ 7

2.2 Barium ................................................................................................ 8

2.3 Lead .................................................................................................... 8

2.4 Chromium ........................................................................................... 8

2.5 Nickel .................... ............................................................................ 9

2.6 Selenium ............................................................................................ 9

2.7 Vanadium ........................................................................................... 9

2.8 Zinc .................................................................................................... 9

3.0 PROOF OF PRINCIPLE TREATMENT RECIPE DEVELOPMENT .............. 10

3.1 Chemical Requirements ................................................................... 10

3.2 Laboratory Equipment Requirement ................................................ 11

3.3 Test Plan for Initial PCP Preparation ............................................... 12

4.0 DATA PLANNING ..................................... i ................................................... 15

4.1 Surrogate Mix Certification ............................................................... 18

4.2 Treatment Recipe Optimization ........................................................ 25

4.3 Process Model Calibration ............................................................... 31

4.4 Treated Product Performance Testing ............................................. 32

4.5 Secondary Waste Acceptance Testing ............................................ 41

5.0 PROCESS DESIGN AND TESTING PROCEDURES .................................. 46

5.1

5.2 Test Procedures ............................................................................... 50

5.3 Process Control Plan ....................................................................... 52 5.4 Test Logs ......................................................................................... 55

5.5 Video Tapes ..................................................................................... 56

Discussion of Design / Configuration ............................................... 46

6.0 EQUIPMENT AND MATERIALS ................................................................... 56 ...... (022498) PL-CNSI-98-004 REV . 0 PAGE 2

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7.0 SAMPLING AND ANALYSIS PLAN .............................................................. 58

7.1

7.2

7.3

7.4

7.5

7.6

7.7

7.8

7.9

7.10

7.1 1

7.12

Sample Objectives ........................................................................... 58

Sampling Methodology ..................................................................... 60

Analytical Methods ........................................................................... 61

Data Quality Objectives and Analytical Support Levels ................... 62

Quality Assurance Requirements ..................................................... 62

Photographs and Videotaping .......................................................... 62

Data Reduction. Validation and Reporting ....................................... 63

Performance and System Audits ...................................................... 65

Operational Evaluation ..................................................................... 65

Calculations of Data Quality Indicators

Quality Assurance Reports to Management .................................... 66

............................................ 65

Corrective Actions ............................................................................ 66

8.0 DATA MANAGEMENT ............................................................... : .................. 67

8.1 Field Activities .................................................................................. 68

8.2 Laboratory Records .......................................................................... 68

Data Handling Records .................................................................... 68 8.3

9.0 DATA ASSESSMENT ................................................................................... 69

. 9.1 Data Validation / Verification ............................................................ 71

9.2 Data Assessment ............................................................................. 72

9.3 Mass and Energy Balance ............................................................... 73

10.0 HEALTH AND SAFETY REQUIREMENTS FOR PROOF OF PRINCIPLE TESTING ACTIVITIES ............................................................. 77

11.0 WASTE STREAM MANAGEMENT ............................................................... 78

12.0 REPORTS ..................................................................................................... 79

12.1 Weekly Teleconferences ................................................................ 79

12.2 Weekly Written Reports ................................................................... 79

12.3 Final Report ..................................................................................... 79

13.0 SCHEDULE .................................................................................................. 81

13.1 Milestones ........................................................................................ 82

13.2 Duration ............................................................. oasm3 .............. 83

. . . . . . . . ,

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14.0

15.0

13.3 Hold Points ....................................................................................... 83

13.4 Witnessing Visits .............................................................................. 83

MANAGEMENT AND STAFFING ................................................................. 83

14.1 Project Management ........................................................................ 83

14.2 Staffing ...................................................... .'.. .................................... 85

14.3 Training ............................................................................................ 85

14.4 Documents ................................. ..;... ................................................ 85

REG U M T O RY COM PLI AN C E ..................................................................... 86

15.1 Licenses ........................... ............................................................... 86

15.2 Permits ............................................................................................. 86

APPENDIX A PROJECT SPECIFIC SAFETY AND HEALTH PLAN ............................ 87

APPENDIX B MATERIAL SAFETY DATA SHEETS .................................................... 88

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1869

1 .o INTRODUCTION

1.1 Project Description

Proof of Principle Testing will be performed at the Chem-Nuclear's Consolidation Facility (CNCF) with Fluor Daniel Femald (FDF) specified Silos 1 and 2 nonradioactive, surrogate slurries. Chem-Nuclear System (CNS) will develop a total of six treatment recipes for these surrogates on a laboratory scale using cement-based stabilizatiodsolidification technology: Resource Conservation and Recovery Act (RCRA) Toxicity Characteristic (TC) and RCRA Universal Treatment Standards (UTS) for Silo 1 surrogate slurry, TC and UTS for Silo 2 surrogate, and TC and UTS for the demonstration surrogate. Only the treatment recipe for TC on the demonstration surrogate sluny will be utilized during the 72-hour demonstration.

Samples will be collected from the laboratory treated surrogates for a TCLP analysis. Demonstration of the process with the demonstration surrogate will be performed over a continuos 72-hour period, and in a minimum of 10 batches. Representative samples of each batch of pre-treated surrogate, in-process surrogate, treated surrogate, and secondary waste streams will be collected in accordance with the Sampling, Data Collection, and Analysis Plan sections of this Work Plan. Samples from the treated demonstration surrogate (final product) will be collected and analyzed for Appearance, Compressive Strength, Free Liquids, TCLP, Dusting/Particulate, and RCRA Characteristics following a 28 days cure period.

Based on CNS's previous experience in using the same cement solidification equipment, adequate and controlled mixing has always yielded a homogenous product. Each batch surface will be inspected for lumps, pockets of unmixed surrogate, and layers.

Following a 28 days cure selected drums (the three batches to be sampled), specified by FDF, will,be cored to collect three one liter samples and the TCLP samples. In addition, a cross sectional core boring will be performed on one of the three drums to verify homogeneous mixing in the 85-gallon drum.

The treated waste/final product will then be profiled for transportation and disposal at a Non-Hazardous Waste landfill.

1.2 Test Objectives

The objective of the laboratory-scale develop,ment of treatment recipes is to identify the remediation recipe that meets the current TC regulatory limits, determine the impact meeting the UTS limits, and optimize waste loading. The goal of the POP testing is to furnish information for the Revised Silos 1 and 2 Feasibility Study and Proposed Plan

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(FS/PP) and as it is intended that the emphasis be on developing an acceptable waste form by CNS using a safe and a reliable process.

2.0 TREATMENT TECHNOLOGY DESCRIPTION

Based upon broad experience in waste treatment for the nuclear industry, Chem- Nuclear has developed cement formula parameters that provide an appropriate starting point as concerns processing the various surrogate compositions. Obviously, the most technically sound and least complicated approach should be first considered, and the following statements better define the scope of the initial lab program.

‘1. flyash promotes excellent reduction of matrix porosity, and provides more fluid bulk mixing characteristics than unmodified cement.

Use of a binder consisting of 65% standard portland cement and 35% class “F”

2. Addition of an hydrous tri-sodium phosphate, if required, should precipitate traces of most polyvalent metal ions (such as lead) that may escape cement matrix entrapment. This additive with a cement-compatible pH has a successful history of use at Chem-Nuclear, and not more than 3% binder replacement is contemplated so that waste loading will be unaffected.

3. 50%) to determine if higher waste loadings may be obtained, contingent upon retaining satisfactory waste form properties (i.e., TCLP values).

Evaluate solidification of wastes at different levels of solids (such as 30% and

The need for any trisodium phosphate in the surrogate solidification formulas has not been established, and the additive is only included with the respect to estimates for the permeability of the cured waste forms. While projected stoichiometric reactions may have some quantitative value, the possible effectiveness of additional phosphate is best demonstrated empirically using a planned set of trial formulas that arbitrarily replace up to 3% of the binder with TSP. However, the appropriate phosphate level should be indicated by the initial TCLP results, and replacement amounts of TSP greater than 3% could then be evaluated if necessary.

Unlike phosphoric acid, trisodium phosphate in aqueous solution tends to buffer pH values in a range conducive to hydration of Portland cement. Also, the dry additive is more convenient to handle, and has a successful use history at Chem-Nuclear.

The ability of properly cured portland cement compositions to retard leaching is well- documented in terms of recorded permeabilities that are comparable to natural stone materials. For example, mineral calcite with a class 10-1 1 permeability is matched by concrete with a water-to-cement ratio of 0.6-0.7. Partial cement replacement with flyash further decreases permeability without increasing total binder weight. Since it is intended to solidify surrogates using water-to-binder ratios less than 0.7, entrapment of toxic metals accounts for more than 99% of the totals present. Chemical precipitation

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of any remaining material is then less than 1% of the totals, and primarily directed toward the control of lead.

Treatment plan CNS proposes will be consistent with that described in the proposal. The proposal addressed each UTS metal and is not repeated in this discussion. It is expected the combinations of the following additives will stabilize all 10 UTS metals: Phosphate, either as phosphoric acid or trisodium phosphate, sodium thiosulfite, sodium sulfide, and ferrous sulfate. The following is a treatment summary: Due to the complexity of the surrogate waste stream(and a review of silos 1 &2 residues composition) CNS may use several chemical additives to stabilize RCRA metals to meet one half TCLP requirements for LDR and to evaluate for meeting UTS. Phosphate, added either as trisodium phosphate or phosphoric acid,. will be used to precipitate lead as insoluble lead phosphate . The solubility of lead phosphate is not pH sensitive as is the case with some sulfates. There are a number of other cautions, both RCRA and non-RCRA metals, that will precipitate as the phosphate (i.e. barium, calcium). Care will be exercised to assure adequate but not excessive amounts of additives are used. Chromium (111) will precipitate as the hydroxide in the presence of sulfide after being reduced from chromium(V1) with sodium thiosulfite. It may be necessary to precipitate nickel and zinc as the sulfide to assure stabilization. Chromium present as a soluble chromate may also precipitate as insoluble lead chromate. Any excess sulfide is precipitated by the addition of ferrous sulfate.

CNS will minimize types and amounts of additives. Chemical types and amounts will be developed during the laboratory phase of the Proof-of-Principle testing.

A maximum of six (6) solidification formulas will be developed in accordance with the established program objectives. This allows for necessary modification of any or all of the three (3) primary formulas meeting one-half of the current RCRA specifications, but failing the generally more stringent UTS limits. CNS has not completed any work yet to support this project. The following is a discussion of the chemical and physical behaviors of metals surrogate constituents to be stabilized:

2.1 Arsenic

Under proposed UTS the TCLP limit for arsenic will not change. TCLP calculations indicate that only about 25% of the waste form arsenic needs to be retained to satisfy limits and therefore, we don't expect any problems. Arsenic is an amphoteric element and exists in different valence states. The valence state can change rapidly and easily with the redox potential. Arsenic should be reduced to the more insoluble trivalent form in order to more effectively immobilize it in a cement-based matrix. The pH of the waste form pore water must be below 11 as arsenic, (111) is soluble above this value. In many cases reduction of valence state is achieved by the addition of either sulfide or sulfite. Arsenic will not interfere with the hydration of Portland cement.

I . .

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2.2 Barium

Under proposed UTS the TCLP limit for barium will be reduced from 100 ppm to 21 ppm. Barium exists in the surrogate as barium sulfate, which is insoluble, and does not appear to require additional treatment. The chemistry of barium is similar to that of calcium and will behave in a similar manner. We do not anticipate any problem with immobilizing barium sulfate in a Portland cement-based matrix.

2.3 Lead

Proposed UTS will change the acceptable lead concentration from 5 ppm to 0.75 ppm. The high concentrations of lead compounds in the waste material relative to the restrictive TCLP requirements allow for practically no release of this element. Tight control of waste form porosity along with additives reducing lead solubility offer the best approach to meeting all requirements. Lead presents the biggest challenge in meeting existing TCLP limits. The more stringent UTS limits will be more difficult to meet. Lead is listed in the surrogate formula as a combination of lead sulfate and lead carbonate. Both compounds have limited solubilities depending upon pH.

The amphoteric nature of lead makes it difficult to immobilize in a Portland cement- based matrix. Lead is fairly insoluble as the hydroxide form between pH 7 and pH 12. Reductive processes can be applicable for improving the retention of lead, even though lead exists only as lead (11). Controlling the pH of the interstitial pore liquid, which in many cases is >pH 12, is an important factor in improving lead retention in a

I cement-based waste form.

Since lead acts as a retardant for the set of Portland cement, we will investigate the use of additives to enhance cementation as part of our formulation development activities.

We also understand that the surrogate contains a source of phosphate. Under certain conditions, soluble lead will react with soluble phosphate to form a very insoluble lead phosphate salt. Patented processes are available that market this type of treatment for municipal and industrial waste.

2.4 Chromium

Preliminary literature references indicated possible problems with cement strength at higher levels of chromium. However, CNS experience at lower levels shows no such difficulty. A review of the surrogate formulas suggest that chromium (as chromates) will combine with lead to form crocoite, an insoluble and stable natural mineral substance that will not interfere with cement set.

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2.5 Nickel

There are no current TCLP limits for nickel. Under proposed UTS, the limit will be 3.6 ppm. Nickel is reported to be chemically bound in a Portland Cement matrix, so that measurable leaching is not expected to take place. Also, only about 50% of the nickel in the surrogate waste form needs to be retained to satisfy the UTS proposed limit. Nickel is added to the surrogate as nickel oxide. When precipitated as the hydroxide, nickel has a solubility of 7x104 mg/L and when precipitated as the sulfide, a solubility of 7 x lo4 mg/L. Nickel does not present a problem for fixation in a cement-based matrix. As with lead, nickel forms an insoluble phosphate.

2.6 Selenium

The treatment standard for selenium is proposed to be raised from 1 .O ppm to 5.7 ppm under UTS. The FDF TCLP limit of 0.5 ppm for selenium is quite low, but control of waste form porosity and use of selective additives should provide satisfactory results. Selenium is added to the surrogate composition as sodium selenite, which is soluble. The Handbook of Chemistry and Physics lists lead selenite and lead selenide as insoluble in both hot and cold water. The possibility exists for soluble selenium to be precipitated by any soluble lead in the surrogate. Fixation efficiency and impact on cement-based waste form properties will be determined experimentally.

2.7 Vanadium

There are no current TCLP limits for vanadium. The proposed UTS limit for vanadium will be 1.6 ppm. Vanadium pentoxide is only slightly water soluble, and at the low concentration in the waste, TCLP values well below the UTS proposed limit are anticipated. Vanadium is added to the surrogate as the pentoxide. As with selenium, the efficiency and impact of fixing vanadium (V) in a cement-based matrix will be determined experimentally. EPA data shows that vanadium waste stream containing 25 ppm vanadium leached 2.006 mg/l. Based on the EPA study, vanadium is not expected to be a problem.

2.8 Zinc

There are no current TCLP limits for zinc. The proposed UTS limit will be 4.3 ppm. Based on the 0.01% zinc oxide in the dry surrogate, the calculated maximum TCLP is only 0.3 ppm which is less than ' 3% of the proposed UTS limit. Zinc is added to the surrogate as zinc oxide.

The effect of soluble zinc present in waste streams is widely discussed in open literature. Soluble zinc has an impact on the two most important mineral phases in Portland cement, tricalcium silicate and tricalcium aluminate. Hydration (setting) of tricalcium silicate is always delayed in the presence of zinc due to the formation of a layer of amorphous zinc hydroxide. It is also reported that when the concentration of

OW003

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sulfate in the cement is above 4.0 %, setting will not occur. The effect of zinc on the hydration of tricalcium aluminate is a function of the sulfate present. Zinc can act both as a set retardant or an accelerator depending upon concentrations of both sulfate and zinc. However, zinc can be rendered insoluble by precipitation to the sulfide form.

It is noted that the surrogate contains a source of phosphate. Under certain conditions soluble zinc will react with soluble phosphate to form an insoluble zinc phosphate compound. This treatment is a patented, commercially available process commonly used to treat both industrial and municipal waste. Again, this encourages the evaluation of cement stabilization additives to fortify the Portland cement-based matrix.

Note that the table on page 11 indicates the degree to which each of these toxic elements must be retained during TCLP testing to conform to both one half RCRA and UTS specifications. It has been indicated earlier that cement matrix entrapment is expected to account for more than 99% of element retention. Therefore, only lead may require additional chemical treatment, and this possibility has been previously discussed in reasonable detail.

3.0 PROOF OF PRINCIPLE TREATMENT RECIPE DEVELOPMENT

3.1 Chemical Requirements

The chemical requirements for the three (3) liter samples of Silo 1 and 2 surrogate wastes are listed below. These are based upon 50% solids, and a 300% safety factor allowing for waste and contingency. Chemical additives with an (*) are water soluble and need not be less than 100 micron powders, since they will be fully dissolved before other items are added. All other chemicals will either be purchased at less than 100 microns or ground and screened prior to surrogate preparations.

NOTE: The handling of hazardous chemicals will follow standard CNS practices as concerns personnel safety. Hazardous chemicals, such as sodium selenite which is poisonous, will be controlled with engineering controls such as a vent hood, in conjunction with goggles, lab coats and properly selected gloves to protect the individuals from hazardous chemicals. Also, once certain toxic substances such as sodium selenite come in contact with other waste constituents, it is very likely that insoluble products will form immediately that will reduce health hazards except for particulate ingestion or inhalation.

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Chemical Name

1 8 6 9

Weight (Grams) for Three (3) Liter Samples

Aluminum Oxide, Al,03 Barium Sulfate, BaSO, (*)Sodium Arsenate, Na,HAsO, (*)Sodium Chromate, Na,CrO, Iron Oxide, Fe,O, Calcium Carbonate, CaCO, (*)Potassium Carbonate, K2C03 (*)Potassium Nitrate, KNO, Magnesium Oxide, MgO Magnesium Carbonate, MgCO, (*)Sodium Carbonate, Na,CO, (*)Sodium Nitrate, NaNO, Nickel Oxide, NiO Vanadium Pentoxide, V,O, Zinc Oxide, ZnO Lead Oxide, PbO Lead Carbonate, PbCO, Lead Sulfate, PbSO, (*)Sodium Selenite, Na,SeO, Tri-butyl Phosphate, TBP Kerosene Diatomaceous Earth, DE Feldspar Coarse Sand Fine Sand Fume Silica Magnesium Phosphate, Mg,(PO,),

54 1,610

18.6*(Note 1 ) 23.4*(Note 1)

732 250.8

12 23.4 24.6

200.4 76.8

139.2 79.8

17 1.8

340 1,668

422 16 (Note 1) 176 (Liquid) 176 (Liquid)

495 2,939 4032 2,424 1,748

308

NOTE 1 : Weight Indicated Allows For Purchase Of Hydrated Form.

3.2 Laboratory Equipment Requirement

Hobart mixer with stainless steel bowl and agitator Grinder Set of 8 inch screens (140,170,200 &235 mesh) with pan & lid (2) dozen PCP cups with lids (1) roll electrical tape screw cap, wide mouth plastic gallon jars (2) screw cap, wide mouth plastic quart jars (1) screw cap, glass pint bottle putty knives and spatulas (1) box heavy duty 1 gallon ziploc bags

.

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(1 ) hammer or mallet (2) dozen wide mouth sample jars to hold 100 gram TCLP sample jars bottle labels marking pens pH meter pH paper, broad & narrow range lab notebook small mortar & pestle (2) eyedroppers several glass beakers, 400 ml, 600 ml, 1000 mi electronic mass balance (1 ) Constant temperature oven

3.3 Test Plan for Initial PCP Preparation

3.3.1 Verify purity of each demo surrogate chemical ingredient and determine as necessary the corrected weights to be added to the mix according to the standard formula.

3.3.2 Verify that the particle size distribution of each dry material is in accord with required values.

3.3.3 Prepare a working quantity of standard surrogate mix at nominal 30% moisture following the POP recommended order of addition of ingredients, and then confirm that the specification of moisture, in-situ density, plasticity, lead TCLP, and pH are acceptable.

3.3.3.1 component in the particular formula that will provide a 3-liter sample of finished material containing 30.0% volatile moisture.

Using surrogate density information, calculate the weight of each

3.3.3.2 In an appropriate container prepare a blend of all dry ingredients.

3.3.3.3 mix thoroughly.

Add the kerosene and tributyl phosphate if required, to the dry blend and

3.3.3.4 any hydrated 3r free water contained in the other 6ormula components.

To the Hobart mixer bowl, add the required amount of potable water less

3.3.3.5 ingredients. Continue mixing until a homogeneous product has been obtained.

Activate low speed mixing, and then gradually add the blend of other

3.3.4 Prepare two PCP master mixes, where BentoGroutTM is dispersed in water and then surrogate added according to the standard formulas shown below. These master mixes will be agitated for at least 24 hours, before individual PCP samples are removed

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and solidified with binder and additives. These PCP samples will then be sealed and weighted prior to cure according to CNS procedure for pozzolanic cement formulas, which spec@ 1-2 days at ambient temperature followed by 4-5 days at 160 +/- 5°F oven temperature.

Master Mixes 30% Solids

Master Mixes 50% Solids

Potable Water BentoGrout” Surrogate Total

NOTE: of cure in a corresponding bulk solidification where normal exotherms are produced because of near adiabatic conditions. Sample curing at room temperature for 28 days does not allow for full strength development, and the practice is only a convenient “rule- of-thumb” for the construction industry. Actually, the measured 28 day compressive strength becomes 35% higher at 90 days cure, and 60% higher after one year. In this respect, bulk solidifications are more consistent in that their exotherms promote reactive full cure in a short period of time.

The specified curing schedule is designed to provide the expected degree

70 parts 50 parts 2.4 parts 4.0 parts 27.6 parts 46.0 parts 100.0 parts 100.0 parts

3.3.5 Prepare corresponding PCP samples from Silo 1 and 2 surrogates by procedure similar to 3.3.1 through 3.3.4.

Example No. Waste Water In Solids ’Naste

(grams) (grams)

1 (30% solids) 30 70 2 (30% solids) 30 70 3 (50% solids) 50 50 4 (50% solids) 50 50

3.4 Performance Assessment

Water/Binder Binder Waste Ratio Weight Loading

weight) ’ 0.7 100 15.0%

0.6 116.7 13.8% 0.7 71.4 29.2% 0.6 83.3 27.3%

(grams) (by

The following table indicates the waste loading range CNS expects to see during testing.

Table 3-1 Sample Waste Loading Calculations Based on 100 grams of water diluted waste

at 30% and 50% Solids

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The following table indicates TCLP requirements associated with the Silo 1 & 2 project. It is assumed that the final waste form is a 50150 weight mixture of binder and additives with waste liquid containing 30 dry solids.

Table 3-2 TCLP Performance Assessment

Dry Wt% Max* FDF UTS Retention** Element COmDOUnd of ComDound TCLP Limit Limit Required

Arsenic Na,HAsO, 0.17 5.1 2.5 5.0 51.0% Barium BaSO, 8.18 361 50 21 94.2% Chromium Na,CrO, 0.27 6.5 2:5 0.85 86.9%

Lead PbCO, 6.60 915 2.5 0.75 99.9%'"""'") PbSO, 2.65 PbO 5.67

Selenium Na,SeO, 0.10 3.4 0.5 5.7 85.3% Nickel NiO 0.43 26 --- 13.6 47.7% Vanadium V,O, 0.09 1.9 --- 1.6 15.8% Zinc ZnO 0.01 0.3 -- 4.3 00.0%

Assuming toxic compound is completely leached. Amount of toxic compound that must be retained during TCLP testing to pass all **

limits.

NOTE: IT IS EXPECTED THAT SOME EXPERIMENTAL LAB WASTE FORM PREPARATIONS WILL EXCEED CURRENT RCRA TOXIC METAL TCLP LIMITS, PARTICULARLY IN THE CASE OF LEAD. DISPOSAL OF SUCH LAB MATERIAL WILL BE ACCOMPLISHED BY CRUSHING TO LESS THAN 4 MESH, AND THEN ENCAPSULATING IN CEMENT PASTE HAVING A W/C RATIO OF LESS THAN 0.5 WHICH ASSURES PRACTICAL IMPERMEABILITY.

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4.0 DATA PLANNING

Three phases of the project data life cycle are addressed in this work plan: data planning, data management, and data assessment. Data planning includes development of data quality objectives (DQOs) and a data collection design. DQOs are qualitative and quantitative statements about the type of data required to provide effective, efficient and defensible answers to the key questions addressed under the POP testing. The project DQOs and data collection design are synthesized into a sampling and analysis plan described in Section 7.0. Figure 4-1 shows the steps in the project data life cycle focusing on the data planning stage.

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Figure 4-1 Project Data Life Cycle: Data Planning Stage

Data Planning Data Quality Objectives and Sampling & Analysis Plan

(Sections 4.0 & 7.0) I

8

I

8

Data Management Field Data Collection and

Associated Quality Assurance/ Quality Control Activities

(Section 8.0)

INPUTS

Data Assessment Data ValidationNerification Data Quality Assessment

(Section 9.0)

I I

I

I

I

8

8

8

8

8

I

8 8

1

a 8

I

I

I

8

I

8

8 I

1 1

Data Quality Objectives Process

Sampling & Analysis Plan

(Section 7.0)

The data management plan provided in Section 8.0 describes how samples are collected and data handled in accordance with quality assurance requirements. Section 9.0 describes the data assessment process utilized to validate/verify data and then to assess data quality relative to the project DQOs. The final step of data quality assessment is to draw conclusions based on statistically treated data to answer the key questions posed under the POP testing.

The DQO process is a strategic planning approach based on the scientific method that is used to prepare for a data collection activity.1 Development of DQOs under EPA guidance involves an iterative, seven-step process:

1 U.S. Environmental Protection Agency, EPA QA/G4. Guidance for the Data Qualib Obiectives Process, EPA/600/R-96/055, Washington, D.C., September 1994.

(022498) PL-CNSI-98-004 REV. 0 PAGE 16 QO()OPki

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0 State the Probkm(s) Identify the Decision(s)

0 ldentrfy Inputs to the Decision(s) 0 Define the Study Boundaries

Develop a Decision Rule(s) 0 Specify Limits on Decision Error(s) 0 Optimize the Design for Obtaining Data

Surrogate Mix Certification

-

The POP testing is necessary to generate data to satisfy data needs in five key areas. These key areas are illustrated in Figure 4-2 and are discussed in detail below.

Process Model Product b Calibration for b Performance

Scale-up Testing A

Figure 4-2 POP Testing Data Needs

4l t- Treatment Recipe

Optimization

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Secondary Waste Acceptance

I Testing I

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A data collection design specifies the final configuration of the monitoring or measurement effort required to satisfy the DQOs. It designates the types and quantities of samples or monitoring information to be collected; what variables are to be measured; where, when, and under what conditions they should be collected; and the QNQC procedures to ensure that sampling design and measurement errors are controlled sufficiently to meet the tolerable decision error rates specified in the DQOs.

4.1 Surrogate Mix Certification

The surrogate slurries must be representative of the Silo 1 & 2 materials and comparable across the four POP vendors. FDF has specified three surrogate formulas for use in the laboratory scale development phase of the project. One of the three surrogate slurries (the demonstration surrogate) will be carried forward for treatment during POP testing. The FDF surrogate formulas are provided in Tables A-1 through A- 3 at the end of this Section.

Chem-Nuclear is required to show through lab analysis (elemental analysis and sieve testing) or chemical supplier certifications that each of the chemical compounds in the mix meets FDF specifications for purity and particle size. The FDF chemical compound specifications are provided in Table 4-1. The quantity of each chemical added to the mix must be adjusted to take into account any moisture content or waters of hydration associated with the chemical compounds as received from the chemical supplier. Special note must be taken of chemical compounds with waters of hydration that require temperatures in excess of 105 C for liberation.

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1 8 6 9

Particle size of silica

Table 4-1 Chemical Compound Specifications

be at least 95% pure. Coarse SiO,: 60 to 80 mesh (250 to 175 micron)

Particle size of insoluble chemicals

Particle size of soluble chemicals Assays of the bulk material

Tolerance of assavs

Fine SiO, < 200 mesh (less than 75 micron) Fume Silica 200 to 250 m2/g.

Shall be < or equal to 100 micron with a distribution following ASTM Method. D422 with mesh sizes of USA sieves 80, 120, 140, 170, and 200 (on the dry mixture of the chemical compounds of a surrogate)

Is unrestricted. Any impurity affecting the mass balance and any RCFUVUTS metals greater than 1 % identified through chemical supplier certification or analysis. +/- 5%

Prior to initiating laboratory scale testing, Chem-Nuclear is to prepare each of the three surrogate slurries prepared at 70 wt% solids (30 wt% moisture) for FDF verification testing to ensure that the prepared surrogates are comparable to the actual in situ silo residues. These verification samples will be analyzed by FDF for the parameters identified in Table 4-2. FDF will respond with analytical results to Chem-Nuclear within seven days of receipt of the slurry sample at the analytical laboratory to inform Chem- Nuclear of the results. Once the samples are collected for FDF analysis, Chem-Nuclear may proceed at the risk of having to re-start the testing or demonstration. If FDF determines that the surrogate slurry does not meet the slurry specifications, Chem- Nuclear will be required to either adjust the surrogate slurry or prepare a new batch and repeat any testing previously performed. FDF will have the option to re-sample and analyze the surrogate slurries after adjustmen. or new batch prekaration.

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Table 4-2 Surrogate Mix Verification

In situ Density

TCLP for I;-- I

based on total weight

DS- 1.78 f 0.1 g/cm3 S1- 1.57 f 0.1 g/cm3 S2- 1.73 f 0.1 g/cm3

Plastic limit 45 to 55 wt % moisture (dry weight basis)

Must leach between 650 and 850 ppm lead

9 to 10

- “Method for Laboratory Determination of Water (moisture) Content of Soil, Rock, and Soil-Aggregate” Packing known mass into graduated cylinder until no further compaction can be observed ASTM Standard “Standard Test Method for Liquid Limit, Plastic Limit, and Plasticity Index of Soils” TCLP EPA SW-846 Method 131 1.

pH test

Adding water or drying at between 105 and 11oc

Contact FDF for adjust men t guidance

Adjust the silica fume to fine silica ratio

Contact FDF for adjustment guidance

Contact FDF for adjustment guidance

The lab scale testing and POP demonstration slurries are to be prepared at 30 wt% solids. The surrogate recipe is provided in Table 4-3. In addition to the verification testing for the 70 wt% solids slurries described above, FDF will have the opportunity to collect or witness the collection of independent samples of the chemical compounds and blended surrogate slurries for the 30 wt% solid slurries prior to the initiation of lab scale development and POP demonstration testing.

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Table 4-3 Surrogate Recipe (30 wt% solids)

Dry Bentonite simulating silo Bentonite cap Potable water

2.4 70.0 100.0

The DQOs for surrogate slurry certification are essentially reduced to the prescription of FDF specifications. The data collection design to certify surrogate slurry preparation includes data collection relative to the chemical compounds, prepared 70 wt% solid slurries and the prepared 30 wt% solid slurries. Table 4-4 summarizes the data variables, collection frequencies, and sample locations for data collection.

Chemical compounds used as components of the surrogate mix must meet the FDF chemical compound specifications for purity and particle size listed in Table 4-1. The Chem-Nuclear Team will utilize material certifications provided by the chemical suppliers to determine compliance with the chemical compound specifications. Chemical supplier certifications will be provided to FDF at least two weeks prior to starting lab scale testing. The moisture content of each chemical received will be determined and recorded to allow appropriate adjustments to the amount of chemical to be added to the surrogate mix. If in any case chemical supplier certifications can not be obtained for a particular parameter or chemical, then Chem-Nuclear will collect a sample for laboratory analysis.

A 70 wt % solid slurry sample of each of the surrogate slurries (i.e., Silo 1, Silo 2, and the demonstration slurry) must be prepared and submitted to FDF for verification testing according to the parameters listed in Table 4-2. Note that these samples are 70 wt % solids samples without any addition of BentoGrout". In addition to the FDF analysis, CNS will analyze each dry surrogate mix (prior to the addition of BentoGroutTM and potable water) for particle size distribution. CNS will also sample each of the 30 wt% surrogate mixes (after addition of BentoGrout and potable water ) for elemental analysis.

(022498)

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3 . /.- PAGE 21 ' , PL-CNSI-98-004 REV. 0

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During preparation of each batch of slurry required for the laboratory scale testing and POP demonstration testing, Chem-Nuclear will maintain required laboratory notebooks and batch sheets to document each of the steps in preparation of the surrogate slurry. These records will contain: the surrogate mix being prepared; the formula for the mix; any adjustments in the mix directed by FDF along with the rationale; results from moisture testing; the scale up factors required to produce the desired quantity of prepared surrogate slurry; the actual measured weights of compounds added; the visual appearance of the mix for homogeneity; the water content of the prepared slurry based on testing; and the time the mix is prepared. FDF will be provided an opportunity to either collect or witness collection of samples of the prepared slurry for verification prior to lab scale or POP demonstration testing. Any required adjustments at FDF direction will be fully documented and recorded.

(D22498) ()QOOZZ

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- 1869

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4.2 Treatment Recipe Optimization

Bench scale studies are required to optimize two treatment recipes (one each for RCRA TC and UTS limits) for each of the three surrogate slurries for a total of six optimized treatment recipes. Recipes must produce treated waste forms that meet RCRA treatment standards and FDF specified waste form performance specifications. In addition, the recipes must be optimized with respect to production characteristics impacting on full-scale design and operations. These specifications drive the data needs relative to treatment recipe optimization.

For the optimized treatment recipes FDF has specified that TCLP results from analysis of the treated waste form be less than one half (50%) of the RCRA treatment standards. The TC and UTS treatment standards and associated (50%) performance specifications are provided in Table 4-5.

Table 4-5 RCRA TC and UTS Treatment Standards

Arsenic (As) Barium (Ba) Cadmium (Cd) Chromium (Cr) Lead (Pb) Mercury (Hg) Selenium (Se) Silver (Ag) Antimony (Sb) Beryllium (Be) Nickel (Ni) Thallium (TI) Vanadium (V) Zinc (Zn)

5.0 100.0 1 .o 5.0 5.0 0.20 1 .o 5.0 - -- -- -- -- -

2.5 50.0 0.5 2.5 2.5 0.10 0.5 2.5 - - I

-- I

, -

21 .o 0.20 0.85 0.75 0.20 5.7

0.1 1 0.07 0.02 13.6 0.20 1.6 4.3

In addition to meeting the TC/U must produce final waste forms that meet FDF waste form performance specifications. Some of the waste form performance specifications are to be measured by Chem- Nuclear while others (Le., durability testing) are to be evaluated by FDF. Table 4-6 identifies the waste form performance specifications that must be met by the optimized treatment recipes.

performance specifications, the treatment recipes

s ." -.

(022498)

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Table 4-6 Waste Form Performance Specifications

Contain no free liquids per ANS 55.1

Fine particulate surrogate shall be immobilized so that the treated surrogate disposal package contains no more than 1 wt% of less than 10-micrometer-diameter particles, or 15 wt% of less-than-200 micrometer-

Strength Free Liquids t- Nuclear

Chem- Nuclear Chem- Nuclear

RCRA Characteristics

diameter particles. The treated waste form shall not exhibit a characteristic Chem- of a hazardous waste (per 40 CFR 261.21 to 261.24) nor Nuclear shall treated waste be listed as hazardous waste.

Durability Examples of tests that may be performed by FDF on

FDF has specified the number and type of samples it requires to satisfy the durability testing needs discussed in Table 4-6. These additional sample requirements are provided in Table 4-7 below.

FDF

oooQ2G (022498) PL-CNSI-98-004 REV. 0

treated surrogate include: Leach Immersion Testing; Shrinking Unreacted Core (SUC) Leach Testing; and Wetting and Drying Testing.

PAGE 26

*

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Table 4-7 Sample Geometry and Quantity Requirements for

Treatment Recipe Optimization

Silo 2 Surrogate UTS

Demonstration Surrogate UTS

12 \2x2 cube

12 \2x2 cube

The optimized treatment recipes will be those recipes that meet all of the performance specifications and contribute to a safe, cost-effective, efficient, versatile and robust full- scale design. One of the primary production characteristics impacting on full-scale design will be the waste loading of the final treated waste form. Additional production characteristics that must be considered during development of the optimized treatment recipes include:

0 Percentage and cost of additives, 0 Ease of forming treated waste into over-the-road transport containers, 0 Ease of process - versatility and robustness, 0 Effect of recipe on equipment maintenance, 0 Ability of recipe to routinely meet waste form performance

specifications.

The data collection design to support optimization of six treatment recipes is focused on collection of samples for waste form performance testing. This includes both the testing for RCRA treatment standards and additional waste form parameters described in Tables 4-5 and 4-6. The samples will be taken from treated surrogate produced over a range of treatment recipes that vary both the waste loading and the binder chemicals. \

(022498)'

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The initial range of recipes to be tested will be developed by personnel familiar with the Process Control Program (PCP) developed by Chem-Nuclear to support the stabilization of a wide range of unique radioactive and mixed waste streams. Section 5.0 of this Work Plan describes in detail the Chem-Nuclear PCP protocols and the process design and testing procedures to be used in optimizing the treatment recipes.

Based on the results from performance testing on samples from the initial range of treatment recipes tested, further modifications may be made for each of the six specific recipes to be optimized. Table 4-8 summarizes the data variables, collection frequencies, and sample locations for data collection.

(022498) PL-CNSI-98-004 REV. 0 PAGE 28

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1869 ma--

4.3 Process Model Calibration

Process monitoring and analytical data are required to characterize the stabilization process for the Silo residues to support preliminary design activities for full-scale treatment. Specifically, data are needed to calibrate the mass and energy (M&E) balances for key unit operations and the overall process. The M&E balances will support development of complete process flow diagrams (PFDs) for full-scale .

operations. The M&E balances and the PFDs will support equipment sizing, duty cycle determination, and development of instrument and control requirements for the full- scale plant. They will also serve as the basis for development of required piping and instrumentation diagrams and will be used to support plant optimization.

The POP demonstration, which will take place at the CNCF, will virtually duplicate the standard full-scale process. The similarities between the demonstration scale and full scale operation facilitate development of balances that can be used to accurately predict and confirm the stabilization technology and its ability to produce a treated waste form that meets all of the performance and acceptance criteria. Data collected to satisfy the M&E balances must be sufficiently precise and accurate to support full-scale design. Uncertainties in measurement of physical parameters (e.g., weight and volume) will be estimated by considering measurements to have an accuracy of +/- 1/2 of the smallest demarcation used in completing the measurement. For example, the uncertainty associated with a volumetric measurement using a calibrated vessel with 0.5 gallon demarcations would be +/- 0.25 gallons. Uncertainties associated with laboratory analysis of chemical parameters will be evaluated using the statistical analyses in combination with the QNQC data collected under the sampling effort.

Uncertainties related to the full-scale operation will be addressed in the Final report. Operational problems encountered during the POP demonstration will be discussed in Section 5.0 of the Final Report. This will include a discussion of how any operational problems encountered during the POP demonstration would be resolved for full-scale design. Key assumptions required for preliminary design, including required allowances for uncertainty, will be discussed in Section 6.0 of the Final Report.

Figure 4-3 shows a simplified process flow diagram for the stabilization process and identifies key sampling/monitoring locations. Table 4-9 identifies the proposed sampling points, parameters, frequency and QNQC requirements. Most of the samples are either grab samples or field measurements/monitoring. The Chem-Nuclear stabilization process is operated in a batch mode. The individual drums produced from the 72-hour demonstration run will be grouped sequentially into ten (1 0) batches each containing approximately the same number of drums.

(D22498) ' . .

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4.4 Treated Product Performance Testing

Data are required to show that the Chem-Nuclear stabilization process can convert untreated Silos 1 and 2 surrogates into a treated waste form that meets waste acceptance criteria. Treated waste forms must meet the RCRA treatment standards specified in Table 4-5. In addition, the treated waste must meet the waste form performance specifications provided in Table 4-6. The process must be able to consistently produce good product over a minimum of 10 distinct batches during the 72- hour demonstration period.

For the 72-hour POP demonstration, samples required for treated product performance testing will be collected from location 6A on Figure 4-3. One complete set of samples will be collected for each of the batches by Chem-Nuclear. In addition, Chem-Nuclear will randomly select samples from three batches and analyze them for the parameters in Tables 4-5 and 4-6. FDF will either concur with the three samples selected by Chem- Nuclear or randomly select an alternate set of three samples. Chem-Nuclear will supply samples of the treated product from the three batches for FDF to conduct durability testing. The sample requirements for FDF durability testing are provided in Table 4-10. Chem-Nuclear will provide FDF with archive samples of treated product from the remaining batches when the final report is submitted at the conclusion of the study. Table 4-1 1 summarizes the required sampling and analysis to meet DQOs for performance testing of the treated surrogate slurries.

The 72-hour POP test will produce ten batches of approximately the same number of drums of stabilized surrogate. The total number of drums produced will be determined after the treatment recipe is optimized at the laboratory scale. If, for example, 50 drums are to be produced, then each batch will comprise five drums. Similarly, if 45 drums are to be produced, then five batches will comprise 5 drums and five batches will comprise four drums. To verify treated product performance, Chem-Nuclear will randomly select samples of treated product from three of the ten batches for performance testing. FDF will either concur with the three samples selected by Chem-Nuclear or randomly select an alternate set of three samples. The cube and cylinder samples for the 72-hour POP test, including samples for compressive strength testing, will be collected wet, following mixing of the final product in the 85-gallon drum, and then oven cured. The oven cure will be conducted at a temperature similar to that realized in the drum core during curing in the 85-gallon drum. The remaining samples, including the TCLP and 3-liter archive samples, will be cored from the 85-gallon drums of cured final waste product.

(D22498) -

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4.5 Secondary Waste Acceptance Testing

The Chem-Nuclear stabilization process is anticipated to operate at sufficiently high solids loadings to allow for partial dewatering of the 30 wt% solids slurry feed prior to stabilization. During full-scale operations the water will be recycled to the extent practicable for use in re-suspension or re-slurrying of residue from the tank transfer area (TTA) to the treatment facility. Waters that can not be recycled or reused in the process will be candidates for disposal at the FEMP Advanced Waste Water Treatment ( A M ) facility. Wastewaters generated during the POP demonstration will be tested to verify that they comply with the AWWT acceptance criteria specified in the Proof of Principle Interface Design Basis document (40720-DC-0001, Revision 0).

Data are required to characterize any wastewater streams that may be produced as a result of slurry feed dewatering. This characterization data will be used to determine what, if any, pretreatment may be required in order to release wastewaters for processing in the A M . Pretreatment requirements and viable technologies to produce a waste stream acceptable at the AWWT will be included in the preliminary design package required as part of the final report. It is anticipated that wastewater pretreatment requirements will be similar to those established for operation of the vitrification pilot plant (VITPP) which was designed for treatment of both surrogate and actual residues. Pretreatment at the VITPP included multimedia filtration for particulate and air sparging to strip radon from the wastewater. The need for additional pretreatment (e.g., precipitation and filtration) will be discussed in the final report based on engineering evaluation of the results obtained from POP testing and the acceptance criteria for the A M . Tat;!e 4-12 provides a preliminary list of parameters that must be addressed in considering wastewater acceptance at the A M .

Additional secondary waste stream, as discussed in section 11.1 of the work plan, will be disposed of at a RCRA TSD facility or applicable landfill.

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Hazardous Waste Total Suspended

Wastewater flow rate pH (electrometric)

Solids (TSS)

10 gpm maximum flow rate

Discharge may not upset treatment operations at the AWWT

Specific Constituents

Table 4-12 Secondary Waste Acceptance Testing

No characteristic or listed hazardous waste No TSS in excess of 1000 ppm.

0 Arsenic (As) 0 5.0 ppm Barium(Ba) 100.0ppm

0 Cadmium 0 1.0 ppm (Cd) 5.0 ppm Chromium 0 5.0 ppm (Cr) 1.0 ppm Lead(Pb) 0 1.0 ppm

0 Selenium

iron (Fe) (se)

(D22498)

The sampling and analysis or monitoring requirements are provided in Table 4-9 under sample location 3A, Dewater Tank.

oo0~42 PL-CNSI-98-004 REV. 0 PAGE 42

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- 1869 Table A-1

Demonstration Surrogate Formula

-.

B~SO, Na,CrO, Fe203

Mg3(P04)2 NaNO, NiO PbO PbCO, PbSO, Na,SeO, Course Si02 Fine SiO, Fume Silica

ZnO Tributyl phosphate Kerosene Diatomaceous earth Feldspar - (Na,K)AISi,O,) H,O

v205

(022498)

186.01 233.40 161.97 159.60 262.88 84.99 74.71

223.00 267.20 303.25 173.01 60.08 60.08 60.08

181.88 81.37

18

8.18 0.27 2.52 2.35 1.03 0.43

6.60 2.65 0.10

19.92 18.90 9.12 0.09 0.01 0.92 0.92 1.83

18.32

100.00

5;67

--

0.12 5.73 0.19 1.76 1.65 0.72 0.30 3.97 4.62 1.86 0.07

13.95 13.23 6.38 0.06 0.01 0.64 0.64 1.28

12.82 30.00 100.00

NOTES: 0 THE DEMONSTRATION MIX IS MODELED AFTER THE SILO 1

RESIDUE, SPIKED WITH SILO 2 CONSTITUENTS. THE 70 WT% SOLID MIX IS INTENDED TO SIMULATE THE ACTUAL IN SITU RESIDUES. ACTUAL CHEMICAL AMOUNTS WILL BE ADJUSTED TO ACCOUNT FOR MOISTURE CONTENT AND WATERS OF HYDRATION IN CHEMICALS AS RECEIVED FROM THE CHEMICAL SUPPLIERS. THREE (3) LITERS OF THE 70 WT% SOLID MIX IS TO BE COLLECTED AND ANALYZED BY FDF. THE DRY MIX IS THE FORMUL 4 TO BE USED F3R ADDITION WITH BENTONITE AND WATER TO MAKE THE 30 WT% SOLIDS MIX.

0

0

0

0

PL-CNSI-98-004 REV. 0 ’ ’ PAGE 43

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Table A-2 Silo 1 Surrogate Formula

Na,Cr04

MgO WCO,

Fe203

K2(C03)2

Mg3(P04)2 Na,CO, NaNO, NiO PbCO, PbSO, Na2Se0, Course SiO, Fine SiO, Fume Silica

ZnO Tributyl phosphate Kerosene Diatomaceous earth Feldspar - (Na,K)AISi,O,) H,O

v 2 0 5

(D22498)

. . . . .. ,

. 233.40 161.97 159.60 138.21 40.31 84.32 262.88 105.99 84.99 74.71 267.20 303.25 173.01 60.08 60.08 60.08 181.88 81.37

18

11.23 0.06 2.90 0.20 0.41 0.73 1.37 1.28 0.53 0.49 16.81 ' 0.00 0.09 23.71 12.27 10.00 0.1 0 0.01 0.00 0.00 1.60 16.21

100.00

7.86 0.04 2.03 0.14 0.29 0.51 0.96 0.90 0.37 0.34 11.77 0.00 0.06 16.60 8.59 7.00 0.07 0.01 0.00 0.00 1.12 11.35 30.00 100.00

NOTES: THE 70 WT% SOLID MIX IS INTENDED TO SIMULATE THE ACTUAL IN SITU SILO 1 RESIDUES. ACTUAL CHEMICAL AMOUNTS WILL BE ADJUSTED TO ACCOUNT FOR MOISTURE CONTENT AND WATERS OF HYDRATION IN CHEMICALS AS RECEIVED FROM THE CHEMICAL SUPPLIERS. THREE (3) LITERS OF THE 70 WT% SOLID MIX IS TO BE COLLECTED AND ANALYZED BY FDF. THE DRY MIX IS THE FORMULA TO BE USED FOR ADDITION WITH BENTONITE AND WATER TO MAKE THE 30 WT% SOLIDS MIX.

. . .

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Table A-3 Silo 2 Surrogate Formula

- 1869 L.

Na,HAsO, BaSO, CaCO, Na,CrO,

KNO,

Na,CO, NaNO, NiO PbCO, PbSO, Na,SeO, Course SiO, Fine SiO, Fume Silica

ZnO Tributyl phosphate Kerosene Diatomaceous earth Feldspar - (Na,K)AISi,O,)

W 5

101.96 186.01 233.40 100.09 161.97 159.60 101.11 84.32

262.88 105.99 84.99 74.71

267.20 303.25 173.01 60.08 60.08 60.08

181.88 81.37

18

0.14 7.40 4.18 0.06 6.78 0.39 2.61 1.40 0.00 0.76 0.41

4.38 0.07

23.57 9.23

10.00 0.09 0.01 2.00 2.00 4.82

14.44

-4.38

I

100.00

0.62 0.10 5.18 2.92 0.04 4.74 0.27 1.83 0.98 0.00 0.53 0.29 3.06 3.06 0.05

16.50 6.46 7.00 0.06 0.01 1.40 1.40 3.37

10.1 1 30.00

100.00

Notes: The 70 wt% solid mix is intended to simulate the actual in situ silo 2 residues. Actual chemical amounts will be adjusted to account for moisture content and waters of hydration in chemicals as received from the chemical suppliers. Three (3) liters of the 70 wt% solid mix is to be collected and analyzed by fdf. The dry mix is the formula to be used for addition with bentonite and water to make the 30 wt% solids mix.

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5.0 PROCESS DESIGN AND TESTING PROCEDURES

5.1 Discussion of Design / Configuration

5.1 .I Description of Operations and Equipment

Pilot scale POP testing will entail stabilization of surrogate waste in 85-gallon drums. Surrogate mix will be dewatered to the maximum extent possible prior to solidification. The amount of dewatering will be determined during the Laboratory scale testing. Surrogate mix and binder will be added to the drum using a drum fillhead. Based on CNS’s experience in solidifying waste in both drums and liners (170 or 195 fit”) CNS has experienced excellent correlation between the two systems.

Filters will be installed into the drum, which are representative of the dewatering filter arrangement installed in the full size (200 cubic feet) stabilization liners. The design of the large scale solidification liner with dewatering capability allows for several configurations and types of filters to be employed for dewatering waste material and optimizing waste loading. The filter size and type installed in the drum for the POP testing will have a configuration and relative surface area to container volume in order to support the scale up to the larger production liner.

Drums will roll on a conveyor to the solidification station, the capping station, and the transfer station. The 85-gallon drums will serve as the process container and the final waste container. Surrogate addition to the drum will be controlled by a fillhead that also ccntrols the addition of binder agents, ventilation, dewatering and mixing. The fillhead used during the POP will be similar to those used during full scale solidification. The fillhead rests on the top of the drum and is connected to the waste, binder, ventilation and hydraulic power plant by hoses.

The fillhead is outfitted with a light and a TV camera to allow the operator to see inside the 85-gallon drum, monitor the sluny level, and observe surrogate and binder addition and mixing. Fillheads are also equipped with connections for thermocouple wires to allow the operator to monitor the temperature of the 85-gallon drum’s contents.

The surrogate will be batch prepared in a mixing tank and then pumped to the 85-gallon drum using an air powered diaphragm pump.

An empty drum, without lid and with integral mixer blade, will be rolled via a conveyer under the fillhead.. The fillhead is lowered by a mechanical devicelequipment onto the drum, and the mixer motor shaft and dewatering leg are connected manually. Once the fillhead is secured (by bolting it) on the drum, surrogates will be transferred to the drum. Dewatering of the surrogate will be performed and more surrogate added if required. The amount of surrogate transferred to the drum and water removed will be established by scaling up the stabilization formula developed in the lab scale testing.

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Following completion of surrogate mix addition the hydraulic power plant will be energized and adjusted to the proper mixer blade speed. Proper mixing speed is determined by a qualified operator observing, on the n/ monitor, the mixer blade rotation and the vortex the rotation creates. After 3 to 5 minutes of mixing, binder will be conveyed above the fillhead and dropped via gravity through the hose into the drum. The quantity of binder added is determined by scaling up the formula from the lab scale testing. When more than one binder chemical is required, each chemical is added in a predetermined sequence. A minimum of three minutes is allowed between each chemical addition to allow mixing and chemical reactions. The minimum duration of these mixing periods will be determined during the lab scale testing. Following addition of the final binder chemical, the mixer continues to rotate for a minimum of 20 minutes to ensure thorough mixing. This addition and mixing procedure is a well-established and successful process.

After the mixer is secured, the fillhead will be unbolted and lifted off the drum, the full drum rolled down the line, and a new drum placed under the fillhead and the process repeated. The full drum will be sampled and capped with a curing lid. The curing lid contains a thermocouple and vent connection. The thermocouple wire on the underside of the lid will be dropped into the wet cement and the lid seated and secured on the drum. The thermocouple wire on top of the curing lid will be connected to the temperature monitor-recorder. The vent is connected to the HEPA system. The curing liner will be allowed to cure for a period of 24-72 hours. During the curing process the internal temperature of the drum will be monitored and recorded. Drum capping will be performed after the cemented waste has reached its peak temperature, has cooled to less than 175 O F and the temperature is steadily decreasing.

The POP will be performed using drums.

Once the curing requirements have been met the curing lid will be removed and the final product will be inspected. Visual observations will be made to ensure there is no free standing liquid. Once the inspections are complete the disposal lid will be installed. The drum will be rolled out to a staging area where it is removed from the conveyor and staged for disposal. A Solidification System Flow Diagram Layout is attached as figure 5-1.

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4 5.1.2 Pre-Treatment Requirements

F -. -1869

The CNS process will perform all treatment of the waste in the final disposal container using equipment that will remain in the disposal container, including filters and mixing blades. The only process that removes material from the disposal container is the dewatering process. Any liquid decanted from the waste slurry during the POP will be returned to the dewatering container, this water could be used to prepare the next batch of sluny during the actual solidification of Silo 1 and 2. Chem-Nuclear's testing program will optimize waste loading to minimize the volume of material requiring off-site disposal. This effort includes evaluating a variety of waste-loading formulas and potential additives to enhance loading and meet the stabilization criteria of the RFP.

5.1.3 Testing Methodology -+

Before beginning any waste processing with the Solidification Unit, the CNS operator shall complete the PCP procedure. The PCP solidification information is recorded on a CNS Solidification Worksheet, and used to calculate the quantities of waste and reagents for solidification in 85-gallon drums. A sample shall be solidified prior to drum solidification of waste. If there is no change in the chemical composition of the waste, the drum solidification will be considered reproducible.

Due to the importance of obtaining a representative sample for use in the PCP verification procedure, the contents of the surrogate mixing tank shall be mixed continuously. This mixing will continue during surrogate transfer to the solidification drums. For demonstration surrogate sample that must be taken from the mixing tank, a sample will be taken from the mixing tank re-circulation line.

5.1.4 Secondary Treatment Requirements ->

Data will be collected to ensure that all secondary wastes generated in the treatment process are identified, minimized to the extent practicable, and properly characterized for appropriate recycle or disposal. During POP testing, water removed (dewatered) from the slurry will be stored in a polyethylene High-Integrity Container (HIC), ready to be transferred to an evaporator system pending laboratory analytical results.

The evaporator system is designed to process radiological waste slurries from 1 % up to 15% solids by weight and conce, Arate the slurry to near dryness. After the water is evaporated, the vapor rises into the vapor bodies and the concentrated slurry comes off the bottoms. The system is nominally rated to evaporate 500 Ib./hr water (1 .O gpm).

The waste slurry (feed stream) is pumped to the Evaporator by the Feed Metering Pump. The feed enters the RotothermQ, and vaporizes. The RotothermQ uses steam as its heating medium. The evaporated water vapor, generated by the Rototherm@, flows through a first stage vapor body. This vapor body cont ' s metal demister type

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filters which entrain and remove water particles from the vapodwater mixture. The entrained water gravity flows back to the Rototherm and the vapor is passed into the condenser. With cooling water supplied to ?he tube side, the vapor condenses on the shell side of the condenser. The condensed vapor or "distillate" gravity drains to and is collected in a 100 gallon distillate receiver. The recovered water pump automatically pumps down the receiver and discharges to one of two tanks in the Distillate Storagerrransfer System.

The concentrated waste, termed "bottoms", gravity flows from the Rototherm@ into the Hood and Drum assembly. This assembly is shielded to reduce radiation exposure (not applicable for POP slurry) during the collection of bottoms material and during the subsequent transfer of full drums of bottoms to the drum storage area. Drums will be disposed of at a RCRA TSD facility.

The only other waste produced are filters from the HEPA control unit, personnel protection equipment (PPE), empty bulk reagent packages, and laboratory waste. These products will be stored/stabilized in 55-gallon drums,'and disposed of at a RCRA TSD facility.

5.2 Test Procedures

System Assembly

Connect suction and discharge hoses to the pumps that will be used for waste transfer, dewatering, and liquid chemical addition as required. The waste transfer system will be tested for leakage prior to use by transferring service water.

0 Place the fillhead on an empty 85-gallon drum and engage the hold-down clamps.

0 Install the vent system on the fillhead, if required.

0 Position the dry chemical hopper on the forklift, if used.

Solidification of Particulate and Liquid Waste Other than Oil or Acid

YOTE: identification.

All drums should bc numbered sequentially to ensure positive

0 Connect an air line or hydraulic hoses to the fillhead mixer motor depending on the type motor used. Adjust the service air or the hydraulic unit to obtain the proper mixer speed for the waste being processed.

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CAUTION: When using the hydraulic mixing motor, a second technician shall be in a position to observe processing and secure the hydraulic unit in the event of mixing blade seizure.

NOTE: chemicals if foaming may occur (based on the pcp or past experience) or does occur during the solidification.

Adjust the mixer speed to a minimum when adding the

NOTE: splashing.

The speed should be fast enough to mix without

0 Load the process drum with the required amount of waste and water as determined by the PCP. Enter the amount on the applicable worksheet.

Dry Chemical Addition

NOTE: chemical addition.

Readjustment of the mixer speed may be required prior to and during dry

By use of bag weights or weighing, add the proper amount of dry chemical to the hopper, if used. Position the hopper to the fillhead fitting, connect service air to the hopper shaker. Open the hopper outlet valve and add the required amount of dry chemicals. Repeat this step for each dry chemical required by the PCP. Enter the amounts of each chemical added on the applicable worksheet.

NOTE: Each dry chemical will be added separately and in the order of the PCP.

0 When all chemicals have been added, continue to mix for a minimum of 20 minutes or until the proper consistency is achieved, whichever is greater.

0 Slowly decrease mixer speed to 0

Securing. the Fillhead

0 Remove and bag the dry chemical addition hopper.

0 Loosen the fillhead clamps and lift the fillhead. Bag the fillhead to prevent the spread of contamination.

Move the fillhead to another preloaded process drum. Remove the bag from the fillhead and repeat steps above.

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0 If no other solidifications are scheduled, clean the fillhead, and store the fillhead on an empty 85 gallon drum.

0 Solidification System Disassembly

0 Remove the fillhead from the drum. The fillhead will be thoroughly cleaned of all chemicals, bagged and mounted on a drum.

0 The drum solidification unit including hoses, valves, etc., shall be decontaminated and released by the CNS's Health Physics personnel prior to storage.

0 All pumps will be flushed or drained as necessary and stored.

NOTE: noted defects will be corrected or replacements ordered.

All hoses and cables will be inspected for defects prior to storage. All

0 All pumps will be flushed or drained as necessary and stored.

The forklift is stored for shipment, including charging of the battery, if required.

0 The dry chemical addition hopper is cleaned and stored.

0 The hydraulic power supply is stored and secured.,

Records and Reports

0 Confirm that the Solidification Records are in compliance with Section 2.4.2 of the QA Plan.

0 Copies of all Daily Operation Logs and Worksheets shall given to the Project Manager, with the technician maintaining a controlled file of worksheets.

5.3 Process Control Plan

CNS Procest Control Program (PCP) is based 0:. Waste Form Certification Program (WFCP) which was instituted to ensure compliance with the IOCFRG? stability requirements for every stabilized solidification performed by CNS. The program is periodically audited through CNS Quality Assurance Program. The WFCP is used to test a specific stabilization formulation based on waste type.

5.3.1 Control Limits

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- 1869 PJ-

CNS cement solidification process is comprised of several processing subsystems, each controlling a specific function of the solidification process. The subsystems include waste transfer, chemical addition, dry material conveyer, hydraulic / mechanical mixer, vent, and dewater systems. Control functions for the unit are incorporated into the pneumatic and electric control panels.

Most of the process components are arranged on portable frameworks to provide flexibility of operations for either indoor or outdoor use. The conveyer system, control panel, hydraulic skid, and fillhead contain most of the major elements of the solidification process.

A closed-circuit television system is an integral part of the fillhead and allows the operator to remotely monitor the solidification process.

5.3.2 Operating ParameterslDeviceslDetectors

The binder agents react with water and with the waste to form solidified stable chemical compounds and hydrates meeting burial criteria requirements. CNS will determine expected thermal effects throughout the solidification process, and will regulate the amounts of binders and additives accordingly to ensure process safety and efficiency.

The Proof of Principle Testing will demonstrate the balance between optimal waste loading and processability of the waste stream. The following define the POP Testing demonstration target parameters:

0 Duration - demonstration of the process with the demonstration surrogate will be performed over a continuous 72-hour period. Unplanned downtime greater than 3.5 hours will require restart of the demonstration and new 72-hour demonstration period.

Quantity - demonstration will process, at a minimum, approximately 2600 kg of the surrogate slurry (30 wt%) solids during each 24-hour period.

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Batches - POP Testing will be performed in a minimum of 10 batches to obtain sufficient data.

0 Samples - during POP Testing, representative samples of each batch of pre-treated surrogate, in-process surrogate, treated surrogatei and secondary waste streams will be collected. CNS will select three samples and submit them for TCLP analysis. FDF has the option to either randomly select the three samples Qr concur on the three samples CNS randomly selected.

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0 Analysis - samples will be analyzed physically (appearance, compressive strength, no liquids) and for TCLP, and RCRA Characteristics to show that the final product meets the acceptance criteria requirements.

0 Process - POP Testing will be performed in 85-gallon batches which can be scaled up to our standard liner sizes of 120 to 195 cubic feet.

Equipment - POP Testing equipment will be representative of the equipment that would be utilized in a full-scale remediation facility.

Curing time of the final product (for the demo) will be 28 days as requested by FDF. During the curing process, drums will be vented and the internal temperature of the drums will be monitored and recorded.

The control system indicates detector components such as:

Waste Valve Control and Position Indicator;

0 Liner Temperature Monitor;

Mixer Speed; and

0 Transfer System Pressure,

The vent stream will be equipped with a HEPA filter and monitored for temperature and relative humidity. Temperature and moisture are the only two parameters of concern that need to be monitored to generate data to show conformance with the design requirements for off-gas to the Radon Control System (RCS) in accordance with the POP Interface Design Basis document (40720-DC-0001, Revision 0). Under full scale processing the vent stream must be controlled to ensure that radon emanating from the treated product is collected and properly treated in the RCS. There are no other constituents of concern in the vent stream that impact on the RCS. Further, there are no constituents of concern or any significant mass that could impact on the overall mass balance for the process.

5.3.3 Monitoring Frequency

Equipment Monitoring

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1869 m-

During drum solidification there will be a continuous monitoring of the processing equipment through a Control Panel. The control system indicates system conditions, alarm conditions and interlocks for various equipment and control system components:

Electrical controls and indications include:

Control Power On, Waste Level Indication, Hi-Hi Level Alarm, TV Camera Light, Waste Valve Control and Position Indicator, Transfer System Controls, Load Cell Readout and Controls, Hydraulic Power Supply Controls, Main Air Controls, Fillhead Vent System Controls,

’ Camera Lens Flush Controls, Hydraulic low oil level alarm, Mixer Speed Control, Dewatering Pump Controls, Emergency Stop, Liner Temperature Monitor, Air Cannon Controls. The pneumatic controls and indicators include: Main Air Pressure, Transfer System Pressure, Dewater Pump Air Pressure Regulator, Camera Lens Air Flow Control, and Fillhead Cooling Flow Control,

ChemicaKPhysical Monitoring

The sampling points, parameters, frequency and rationale for selection is discussed in detail in sections 4.0 and 7.0 of this Work Plan.

5.4 Test Logs

Treatment recipes tested, will be documented along with testing and evaluation of the resulting batch of treated surrogate. CNS chemist will record and justify adjustments to the treatment recipes in laboratory logbooks.

CNS will submit to FDF all batch sheets, analytical data packages, testing logs, and laboratory notebooks pertaining to the Proof of Principle Testing findings. Testing documentation will be submitted to FDF as an attachment to the final report.

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5.5 Video Tapes

CNS will videotape the 72-hour process demonstration. In addition, the video taped demonstration will be operated at a production rate that will provide FDF confidence that the process can be scaled-up to treat the Silos 1 and 2 residue during 36 months of operations. Videotapes will be forwarded to FDF with the draft final report.

6.0 EQUIPMENT AND MATERIALS

The following provides a listing of the type and quantity of equipment that will be required to complete the POP testing. This list is subject to modification, addition and deletion during the system design and lab scale test phases of the project.

A. Conveyor 1. Straight sections, 2. 90' sections, 6 3. Supports, 24 4. HEPA Hoses, 40

B. Fillhead 1. Hydraulic system, ;3 2. Solidification Fillhead, 1 3. Hoses (hydraulic), 2 4. 5. Plant Connection Stand, 1

Control Panel (Drum wml), 1

C. Cement System I. Auger, 1 2. Dust control, 1

D. Surrogate waste System 1. Mixing container, 2 2. 3. Hoses (hydraulic), 4 4. Pump (2 inch), 3 5. Hose, 6 6. Mixer Head, 2 7. Dewatering container, 1

Control Panel (mixing tank), 2

E. Consumables 1. Drums, 55 2: Curing Lids, 55 3. 4. 5. Mixing Blades, 55

Computer, 1 (not a consumable) Temperature Monitor (32 station), 1

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6. Modify Drums for Dewatering/Solidification, 55

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7.0 SAMPLING AND ANALYSIS PLAN

This Section of the Work Plan describes how the required sampling and analysis and monitoring are carried out in accordance with project DQOs. It also identifies those sampling and analysis activities that are driven by the Chem-Nuclear Quality Assurance Program requirements .

7.1 Sample 0 bjectives

Sufficient data will be collected during laboratory bench scale and POP demonstration testing to provide an effective, efficient, and defensible description of the Chem-Nuclear solidification process and its performance relative to Silos 1 & 2 materials. Data generated under this sampling plan will satisfy project DQOs relative to: surrogate slurry certification; treatment recipe optimization; process model calibration for scale-up; product performance testing; and secondary waste acceptance testing. The data needs relative to each of these areas and the project DQOs are discussed in detail in Section 4.0 of this work plan. Table 7-1, presented at the end of this Section, summarizes the sampling and monitoring required to support the POP demonstration. With an understanding of the data needs at the outset of the project, the data collection program is structured to ensure that data of the right type and quality are collected to answer key questions in characterizing the process.

7.1.1 Surrogate Slurry Certification

Data will be collected to demonstrate Chem-Nuclear conformance with the FDF specifications for the surrogate slurry preparations to be used in this study. Specifically, Chem-Nuclear will collect data for the component chemical compounds, the prepared 70 wt% solid surrogate slurries, and the 30 wt% solid surrogate slurries. Conformance with the specifications will ensure that POP demonstration results are comparable across POP vendors and that project results are defensible.

7.1.2 Treatment Recipe Optimization

Two treatment recipes will be optimized for each of the three surrogate slurry mixes (Silo 1, Silo 2 and demonstration slurry) for a total of six optimized treatment recipes. Each treatment recipe will have to produce a final waste form that satisfies a RCRA treatment standard specification (i.e., one-half the TC or UTS) as well as treated kroduct performance specificatior IS. Each treatment recipe v~ill be optimized relative to production characteristics impacting on full-scale design and operations. One optimized treatment recipe for the demonstration slurry will be carried forward to the 72- hour pilot scale POP demonstration testing. Data collected under this sampling and analysis plan will document the approach used to develop each of the optimized treatment recipes.

. .

7.1.3 Process Mbdel Calibration for Scale-up

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- 1869 -- -

Data collected under this’sampling and analysis plan are required to calibrate the process models for the solidification of the Silos materials to support preliminary design of the full-scale remediation process. The POP test program is also concerned with generating objective evidence that the solidification process can be readily implemented and reliably produce competent treated waste. The Chem-Nuclear solidification process lends itself to scale-up using essentially the same equipment and processing geometries that would be used in full scale processing. Demonstration process will run at a speed to represent full-scale processing. Data will be collected to complete mass and energy balances about the mixing and curing operations, as well as overall mass and energy balances.

In addition, during the 72-hour POP testing, data will be collected to show the time evolution required for each process step. The entire 72-hour POP demonstration will be video taped, supporting analysis of time/motion in the treatment process. This information will facilitate preliminary design work for required layout of the full-scale remediation facility (e.g., required curing facility and final product inspection/storage capacity). This data will also be useful in projecting cost and schedule implications for full scale processing.

7.1.4 Product Performance Testing

Data are required to demonstrate that final treated product from the solidification process meets FDF performance specifications. The final product must pass the RCRA treatment standards and meet certain minimum waste form specifications. In addition, production characteristics that will impact on full-scale design and/or operations will be monitored during the test cycle. For example, waste loading in the final treated product is a very important production characteristic that will have significant impact on full- scale production design and cost estimates. Much of the performance testing is to be completed by Chem-Nuclear, although FDF is responsible for specific durability testing.

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7.1 -5 Secondary Waste Acceptance Testing

Data will be collected to ensure that all secondary wastes generated in the treatment process are identified, minimized to the extent practicable, and properly characterized for appropriate recycle or disposal. During POP testing, water removed (decanted) from the surrogate will be the most significant secondary waste generated. At full-scale processing, this stream will either be recycled for use in hydraulic transfer of slurry or will be tested (and treated if necessary) for release as wastewater. Other secondary waste forms include personal protective clothing/equipment, HEPA filters, and bulk chemical packaging from binder chemicals. At full-scale processing, all equipment will be maintained under negative pressure with the exhaust drawn from the process directed to the Radon Control System which will provide radon and particulate treatment. At full-scale operations they will be designed to effectively control particulate radionuclides and radon emissions.

7.2 Sampling Methodology

The 72-hour POP test will produce ten batches of approximately the same number of drums of stabilized surrogate. The total number of drums produced will be determined after the treatment recipe is optimized at the laboratory scale. If, for example, 50 drums are to be produced, then each batch will comprise five drums. Similarly, if 45 drums are to be produced, then five batches will comprise 5 drums and five batches will comprise four drums. To verify treated product performance, Chem-Nuclear will randomly select samples of treated product from three of the ten batches for performance testing. FDF will either concur with the three samples selected by Chem-Nuclear or randomly select an alternate set of three samples. The cube and cylinder samples for the 72-hour POP test, including samples for compressive strength testing, will be collected wet, following mixing of the final product in the 85-gallon drum, and then oven cured. The oven cure will be conducted at a temperature similar to that realized in the drum core during curing in the 85-gallon drum. The remaining samples, including the TCLP and 3-liter archive samples, will be cored from the $5-gallon drums of cured final waste product.

The proposed sampling points, parameters, frequency and rational for selection were discussed for each of the five main data needs areas of the project in Sections 4.1 through 4.5. The process sampling points are identified schematically on Figure 4-3. Table 7-1 summarizes the sampling and monitoring required to support the POP demonstratior;. Most of the samples to be collectd are either grab samples or field measurementslmonitoring. The rationale for selecting these proposed sampling points directly relates to the data needs associated with the DQOs and sample objectives described above. The Chem-Nuclear stabilization process is operated in a batch mode. The individual drums produced from the 72-hour demonstration run will be grouped sequentially into ten (q 0) batches each containing approximately the same number of drums.

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Y.

Sample analysis request and custody record (SAWCR) forms will be prepared prior to sampling to facilitate field collection of samples. Sample containers will be purchased pre-cleaned in accordance with EPA SW-846 specifications with appropriate supplier documentation and unique container identification. As samples are collected in accordance with the sample request form, the collected samples will be entered on the SAWCR form.

The SAWCR form will also be used to record required field preservation and sample handling requirements. The SAWCR form will identify those QA samples that must be collected in order to satisfy QA requirements. The chain-of-custody process will be conducted in accordance with €PA sample custody protocols described in NElC Policies and Procedures, EPA-330/9-78-001 -R. Chain-of-custody will be maintained from sample collection and handling in the field through laboratory receipt and analysis and will be properly documented in evidence files.

Data collection activities will be recorded in a bound field log. Activities documented in the log will be described sufficiently for the sampling team to reconstruct a particular situation without reliance on memory. Logbook pages will be sequentially numbered and identified by a project-specific control number.

Samples will be handled, packaged, labeled and shipped in accordance with Federal and state regulations pertaining to shipment of environmental samples and hazardous materials. Chain-of-custody procedures will be maintained throughout the shipping process with appropriate chain-of-custody seals placed on the exterior of sample packages.

7.3 Analytical Methods

Field measurements and monitoring will be conducted according to ASTM method and/or Chem-Nuclear procedure. Laboratory analysis methods will be conducted in accordance with FDF approved laboratory procedures at the FEMP SCQ approved General Engineering Laboratory of Charleston, South Carolina. This will ensure that data collected and analyzed in support of POP testing will be of sufficient quality to facilitate their use as support data under the Revised Silos FS/PP (Feasibility Study/Proposed Plan).

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7.4 Data Quality Objectives and Analytical Support Levels

Data Quality Objective (DQO) analytical levels are defined in the US EPAs “Guide for Conducting Feasibility Studies under CERCLA”. This guide states that the requisite analytical levels are dictated by the types and magnitudes of decisions to be made based on the data and the objectives of the screening. Section 4.0 of this Work Plan provides a more detailed discussion of the Project DQOs and data collection design utilized to satisfy these DQOs.

The DQOs are qualitative and quantitative statements that specify the quantity of data required to support the decision making. DQOs are based on the end use of the data to be collected. For analytical measurements, this study will utilize the five FEMP- defined analytical levels defined by the SCQ. These levels (A through E) are analogous to the 1987 EPA defined DQO levels 1 through 5. ASLs will be assigned depending on the intended use of the data and the Quality Assurance/Quality Control methods required to achieve the desired level of quality.

Analysis which are direct instrument readings are assigned an ASL level of “A. Level B is appropriate for most analysis in this study, because it will allow user defined and special requirements. Where more stringent analytical level are required, the analytes are assigned an ASL of “C”. Based on the assumption that data from the chemical composition analysis of the TCLP leachate during the POP test will be used to support the Revised Silos FS/PP (Feasibility Study/Proposed Plan) effort, they were assigned an ASL level of “C”. These analyses will be performed at an SCQ-approved laboratory. Box 7-1 provides additional description of the ASLs used on this project.

7.5 Quality Assurance Requirements

Quality assurance will be conducted in accordance with the Project-Specific Quality Assurance Plan and Chem-Nuclear‘s Quality Assurance (QA) Program (QA-AD-001). The Project-Specific Quality Assurance Plan is designed to be consistent with the requirements of the FEMP SCQ to the extent possible. For example, as discussed above, the project is utilizing the same ASLs defined under the SCQ. Laboratory analysis work, including required QNQC procedures, will be conducted at the SCQ- approved General Engineering Laboratory in Charleston, South Carolina. The laboratory will generate data packages in essentially the same format as those produced for the FEMP under the same ASLs. This accommodation will ensure that laboratory data generated under the project will be comparable not only in quality, but also in format, to typical data sets generated in support of FEMP projects.

7.6 Photographs and Videotaping

Still photography and video taping of testing activities will be used to document the processes and procedures involved as well as the techniques involved in the

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- --- 1869 demonstration of the stabilization technology. For all photographs taken, a photographic log will be maintained and will include the date, time, and description of photograph, location, direction of photograph, photographer, and frame and film roll number. For video taping, audio documentation (narrative) will be used to provide descriptions of locations and processes. The date and time will be automatically displayed on the tape.

7.7 Data Reduction, Validation and Reporting

Data reduction, validation and reporting will be completed as applicable for the ASL Level specified for each sample analysis. The process for data management is detailed in Section 8.0 of this Work Plan. Data reduction involves the converting of raw data to a useable format. Data reduction will be completed by the laboratory analyzing the samples or field personnel responsible for obtaining field measurements. Where required, data validation will be completed in accordance with the discussion in Section 9.0 of this Work Plan by personnel independent of the laboratory or field personnel generating the analytical data. The data validation process provides the required steps for review and qualification (flagging) of the analytical data. Required certificates of analysis and summary sheets will be generated by the analytical laboratory. Field- generated data reports for ASL Level A will include field logs and report forms appropriate to the measurement or monitoring.

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BOX 7-1 Analytical Support Levels (ASLs)

ASL A (Qualitative Field Analvsis) -Provides the most rapid (real or short time) results. ASL A is often used for preliminary comparison to ARARs, initial site characterization to locate areas for fixed laboratory analysis, and engineering screening of alternatives (bench-scale tests). These types of data include those generated on site through the use of photo- or flame-ionization detectors, pH and conductivity meters, alpha and beta/gamma friskers, or radiological swipe samples. Analogous to U.S. €PA DQO Level 1.

ASL B (Qualitative. Semi-Quantitative and Quantitative Analvses) - Provides more quality control checks than ASL A and results may be qualitative, semiquantitative, or quantitative. ASL B can be assigned when rapid turnaround results are needed. FEMP-specified analytical protocols shall be used. There are two sublevels available for specifying QNQC, data reporting, and data validation requirements.

Sublevel 1 specifies QNQC, data reporting, and data validation requirements for FEMP- specified analytical protocols which are similar to those used for ASLs C and D, but with different W Q C sample type and frequency, quality control criteria for acceptance ranges, and requirements for data packages.

Sublevel 2 specifies userdefined and special requirements. The data use shall specify QNQC, data reporting, and data validation requirements based on intended data use and regulatory requirements. Specific requirements shall be defined in Project Specific Plans (PSPS).

ASL C (Quantitative with Fullv Defined QNQC) - Provides data generated with full QNQC checks of types and frequencies specified for ASL D (see below) according to FEMP- specified analytical protocols for radiological and nonradiological parameters. The analytical methods are identical to ASL D for W Q C sample analysis and method performance criteria. However, the data package does not typically contain raw instrument output, but does include summaries of W Q C sample results. ASL C may be used when analyses require a rigid, welldefined protocol, but where other information is available so that a complete raw data package validation effort is not required. Laboratories shall be required to retain raw instrument data in the project file required to upgrade ASL C reports to ASL D.

ASL D (Conformational with ComDlete W Q C and RePortinq) - Provides data generated with a full complement of QNQC checks of specified types and frequencies according to FEMP-specified analflcal protocols for radiological and nonradiological parameters. The data package includes raw instrument output for validation of ASL D data. It may be used to confirm data gathered as ASLs B and C and when full validation of raw data is required.

ASL E (Non-Standard) - Analyses by non-standard protocols that often require method development or validation (e.g., when exacting detection limits or analysis of an unusual chemical compound are required). ASL E methods may be significantly different from those specified for ASLs B, C, or D data. New methods may be developed for ASL E data to allow for parameters of matrices that cannot be analyzed using existing standard methods. This could be caused by interferences, analyses performed outside of accepted requirements for existing methods, or new methods developed to meet site requirements or project-specific requirements that cannot be met by existing analytical methods.

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7.8 Performance and System Audits u-- 1 8 6 9

Self-assessments and independent assessments of work processes and operations will be undertaken to ensure quality of performance under the project. Independent assessments will be conducted under direction of the QNQC Manager. Self- assessment will be performed under the direction of the Chem-Nuclear Project Manager. Audit and surveillance performance will be controlled under the Chern- Nuclear QA Program (QA-AD-001 Section 18.0) and the Project-Specific Quality Assurance Plan for POP Testing.

7.9 Operational Evaluation

During the testing program, sampling and analysis personnel will be interviewed by QNQC Manager to obtain an overview of the S&A aspects of the testing operations. This evaluation will be performed at least once during each phase of the testing (surrogate preparation, treatment recipe development, POP demonstration testing, and product and waste sampling) and will be performed soon after sampling activities have begun (Le., before one-third of the samples have been collected and analyzed). The evaluator will observe sample collection, sampling documentation, labeling, measurement, calibration and data recording procedures.

7.1 0 Calculations of Data Quality Indicators

Sufficient quality indicators will be collected to provide a means for assessing data precision, accuracy and completeness. Section 8.0 of this Project Work Plan describes the means for retrospective assessments of the quality of results from the data collection efforts. These assessments will help verify that the data are of sufficient quality to satisfy the objectives of the project. In addition, this Section discusses the statistical methods to be used for handling and interpreting data for decision-making purposes. The EPA Guidance for the Quality Assessment: Practical Methods for Data Analysis (EPA QNG-9) will serve as the basis for selecting assessment methods. Data may be treated statistically using the EPA DataQUEST software or an equivalent commercial package.

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7.1 1 Corrective Actions

Assessments of project quality will include identifying deviations, correcting the source of the deviations, and verifying that corrective actions have been implemented. Corrective action for problems will include, to the extent possible, identifying root causes of problems and procedures to prevent their recurrence. Corrective actions will be implemented, as necessary, in accordance with the Chem-Nuclear QA Program (QA-AD-001 Section 16).

7.12 Quality Assurance Reports to Management

Quality Assurance reports to management will be submitted in accordance with the Chem-Nuclear QA Plan (QA-AD-001).

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8.0 DATA MANAGEMENT

The data management process is designed to track the path of data from their generation in the field of laboratory to their final use or storage. Data records and documentation may be generated during field activities, laboratory analysis, or subsequent data handling activities. Figure 8-1 shows the relationship of data management activities to the overall project data life cycle.

Data Planning Data Quality Objectives and Sampling & Analysis Plan

(Section 4.0 & 7.0)

Figure 8-1 Project Data Life Cycle: Data Management Phase

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Field Activities Sampling Records

+ Container certification + Chain-of-custody forms + Field log book

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Monitoring Records + Instrument calibration + Manual data logs + Automated data logs

Analysis Records + Chain-of-custody forms + Routine data + QC I Perfomance data

Analysis

Data ValidationNerification + verify measurement performance + Verify measurement procedures Data Assessment

Data ValidationNerification Data Quality Assessment

(Section 9.0)

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8.1 Field Activities

The information contained in these records documents overall field operations and generally consist of the following:

Sample collection records: These records show that the proper sampling protocol was performed in the field. Key information contained in the sample collection records includes: the names of the persons conducting the.activity, sample number, sample collection points, schematics and diagrams, equipmenVmethod used, climatic conditions, and unusual observations. Sample collection records are maintained in bound field notebooks as well as on the sample analysis requestkustody records (SAWCR). In addition, field records may be contained in manual or automatic data

.

logs.

Chain-of-custody records: The chain-of-custody record documents the progression of samples as they travel from the original sampling location to the laboratory and finally to their disposal area.

QC records: These records document the generation of QC samples such as field duplicates. They also include documentation on sample integrity and preservation and include calibration and standards' traceability documentation capable of providing a reproducible reference point. Process monitoring instrumentation, for example, will be calibrated to nationally traceable standards.

General field procedures: General field procedures record the procedures used in the field to collect data. Chem-Nuclear field activities, such as collection of samples, are implemented under a reference procedure that controls field activities or instructions contained in the project work plan.

Corrective action reports: Corrective action reports document what methods were used in cases where the general field practices or other standard procedures were violated. Corrective action reports include the methods used to resolve compliance and the actions taken to prevent recurrence.

8.2 Laboratory Records

Laboratory records provide documentation relative to laboratory actions that potentially impact upon the quality of the final data generated. Examples of key laboratory records include sample data, sample management records, documentation on test methods, and QNQC reports.

8.3 Data Handling Records

Records generated during data reduction, data validation, and data assessment are part of the data assessment phase of the data management life cycle. Section 9.0

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r- 1869 --- discusses the approach Chem-Nuclear will take relative to these important areas. Software programs (e.g.,' spreadsheet or database programs) will be used to collect data that have been reduced and released for use in the project.

9.0 DATA ASSESSMENT

There are two main steps to data assessment. The first step is to assemble the routine data and QC performance evaluation data from analysis and complete data validation/verification. This is the process of verifying measurement performance and procedures and compliance with recording requirements. The second step is to complete the data quality assessment process whereby the data are evaluated to ensure that they meet project DQOs and then applied to the decision rule make conclusions relative to the key questions posed by the study. Figure 9-1 illustrates the general data assessment phase of this project.

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Figure 9-1 Project Data Life Cycle: Data Assessment Phase

Data Planning Data Quality Objectives and Sampling & Analysis Plan

(Section 4.0 & 7.0) I

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Data Management Field Data Collection and

Associated Quality Assurance1 Quality Control Activities

(Section 8.0)

Data Assessment Data ValidationNerification Data Quality Assessment

(Section 9.0)

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Validated Verified Data

INPUT . Data Quality Assessment

+ Review DQOs and design + Conduct preliminary data review + Select statistical test + Verify assumptions + draw conclusions

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rim- - 1869 --- 9.1 Data Validation / Verification

Chem-Nuclear is using the FEMP SCQ-approved General Engineering Laboratory in Charleston, South Carolina to conduct required analytical testing. Chem-Nuclear will request that the laboratory generate and supply QNQC performance data under the same protocols used for all FEMP sponsored work. Similarly, Chem-Nuclear will utilize the same data validation review forms contained in the FEMP Data Validation Procedure (EW-0010).

Each analytical data release from the laboratory will be reviewed to ensure that all contractual requirements have been met and all required QNQC performance data have been submitted with the data release. Minimum required supporting documentation that should be provided from the laboratory to complete inorganic and conventiona! data validation checklists include the following:

Inorganic Data

Qualified FORM Is (Le., copies of summary result forms containing validation qualifiers) QNQC Summary Forms:

1. CRDL Standard Recoveries (Form 11-2) 2. Blank Results (Form 1 1 1 ) 3. Interference Check Standards (Form IV) 4. Spike Sample Recoveries (Form V-1) 5. Post Digestion Spike Recoveries, if analyzed (Form V-2) 6. Duplicates from the laboratory (Form VI) 7. Standard Addition Results, if any (Form VIII) 8. Serial Dilution Results (Form IX) 9. Instrument Detection Limits (Form X) 1O.Analysis Run Logs (Form XIV)

Conventional Data

Qualified FORM Is (i.e.l copies of summary result forms containing valid at ion qualifiers)

0 QNQC Summary Forms: 1. Calibration verification informa.,on (control sampl;: recoveries if

present) 2. Surrogate, matrix, or lab spike data 3. Lab or field duplicate information

A data validation checklist will be completed for each analytical data release. An example of a data validation checklist for inorganic data may be found in the FEMP Data Validation Procedure, EW-0010, Form FS-F-3806. An example of a data

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validation checklist for conventional data may be found in Form FS-F-3807 of the same FEMP procedure. If necessary, a formal request will be made of the laboratory to supply any missing or illegible information that is required to complete the validation process.

Field collected data will also be subjected to a validation process to evaluate field activities to detect any impact on the reliability of the sample results. Field validation includes checking calibration records of field instrumentation, field logbook, Chain-of- Custody forms and other indices of quality generated during field activities. An example of a field data validation checklist is Form FS-F-3801 from FEMP procedure EW-0010.

Verified and validated data will be input into a database or spreadsheet application to present the data for the data quality assessment process. This electronic copy of the data will facilitate data assessment and application of statistical tools either directly in the databasekpreadsheet or be exporting the data to a data analysis software package (e.g., EPA DataQUEST or a similar commercially available package).

9.2 Data Assessment

The first step in the data assessment process will be to review the project DQOs and ensure that they are still applicable. The rationale will be provided for any changes in either the data collection design or the DQOs. For example if FDF specification is not, in practice, achievable then the justification for variance granted by FDF will be documented. Similarly, if there was a change in the original data collection design (e.g., additional samples deemed necessary or particular sample collection not feasible) then the rationale for the change will be documented. Issues driving changes in either DQOs or data collection design will be promptly communicated to FDF for resolution.

The collected data will be subjected to a preliminary data review. The QA reports will be reviewed, basic statistics for the data computed, and graphs generated (where appropriate) to learn about the structure of the data sets. The preliminary data review will rely on outputs from the data verification/validation process including data validation checklists and database or spreadsheet applications containing data that have been reviewed and released.

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Based on the preliminary data review and the nature of the DQO, an appropriate procedure will be selected for summarizing and analyzing the data. A statistical test may be selected for one or more of the parameters. For others, the data may be used as point estimates to determine compliance with FDF specifications. Where a statistical test is selected for data assessment, any underlying assumptions required for the test to be valid will be verified (e.g., assumptions about normality). Statistical analyses may be completed in a spreadsheet or in data analysis software such as EPAs DataQUEST or a suitable commercial substitute.

Finally, conclusions based on the data will be drawn. Where a statistical test has been selected, the required calculations will be conducted and documented. The inferences drawn as a result of these calculations will be documented and discussed in greater detail in the final report for the project. Where data are being used as point estimates for process parameters (e.g., related to compliance with FDF specifications), the proximity of the point estimate to the critical region for the decision will be discussed and uncertainties implicated in preliminary design of the full-scale process.

9.3 Mass and Energy Balance

An integral mass balance for the stabilization process will be developed based on the principle of conservation of mass. The mass balance will be conducted across the waste liner which serves as the mixingkuring unit. The balance will consider the starting and ending configurations of the system. Figure 9-2 provides a graphic representation of the mass balance. Data collected through sampling and analysis and process monitoring will be used to calibrate the process model.

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mu-- 1869.

An overall mass balance and a constituent balance for RCRA metals will each take the general form:

input - output = accumulation

where: input = feed materials to the system, output = products leaving the system, and accumulation = buildup within the system

The overall mass and RCRA metals balance will ensure that materials are accounted for in the process and provide essential information required for scale-up of the process and preliminary design calculations.

In addition, a balance will be conducted on solids and water in the system. These balances will take the form:

input + generation - output - consumption = accumulation

where: input = feed materials to the system, generation = materials produced within the system, output = products leaving the system, consumption = materials consumed within the system, and accumulation = buildup within the system.

The water and solids balances will provide information required for scale- up of equipment and process controls for full-scale operations. In addition, these balances will be used in determining requirements for secondary waste treatment (Le., for offgas and decant water streams).

An overall or macroscopic energy balance for the stabilization process will be obtained by applying the principle of conservation of energy to a control volume fixed in space. The control volume is the waste liner serving as the mixing/curing unit. The data collected through sampling and analysis and process monitoring will be used to calibrate the energy balance for the stabilization process. The basic energy balance across the control volume may be expressed as follows:

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A H = Q - W ,

where: AH = change in enthalpy of the system

Q = heat transferred across the control surface, and W, = mechanical energy associated with the mixer

The stabilization process is exothermic, creating heat as the surrogate, binders an d water react to form the treated product. The change in enthalpy for the process will be determined empirically by measuring the difference between the heat transferred across the control surface and the work introduced into the system. The heat transferred across the control system is primarily associated with heat directly transferred through convection and conduction. A heat transfer model will be developed to allow the instantaneous heat flux across the surface of the liner to be determined based on the difference between the liner skin and ambient temperatures. integrating the instantaneous heat flux over the curing period will provide an estimate of the heat transferred across the control surface (Q) through convectionkonduction. The energy associated with the shaft work is anticipated to be a small term in comparison to the other energy terms. Process monitoring will be used to estimate total shaft work introduced to the system during the mixing period.

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1869. u--

10.0 TESTING ACTIVITIES

HEALTH AND SAFETY REQUIREMENTS FOR PROOF OF PRINCIPLE

The Project Specific Safety and Health Plan (PSSHP) provides guidance for the proof of principle testing to be conducted at the Chem-Nuclear Consolidation Facility (CNCF). The testing will be conducted in two phases, (1) laboratory (bench) scale testing and (2) pilot scale testing. Each type of testing has been conducted previously at these facilities and the hazards associated with them are well known.

The primary hazard is the potential for airborne hazardous chemicals for example; arsenic, chrome, and lead. Airborne dusts will be controlled via three forms of engineering controls; (1) the central HVAC system which is equipped with HEPA filters, (2) local HEPA air movers which can be positioned near the potential source and (3) water mist to wet the powder preventing it from becoming air borne.

Two specific tasks present the most risk for creating an airborne condition; (1) the sieving process that is used to assure particle sizes for the tests and (2) the actual mixing of the chemical components to make the surrogate waste media. These risks are minimized during the laboratory scale tests because of the volume of material involved. Further, a fume hood is available to contain dusts during the sieving task. The sieving and chemical mixing task during the pilot scale testing will require the use of respiratory protection.

Physical hazards to be considered are consistent with an industrial work area. They include pinch points, falling objects, burns, cuts, and muscle strains. These hazards will be controlled using safe work practices, engineering controls and personal protective equipment. 1

A detailed Project Specific Safety and Health Plan (PSSHP) is attached to this Work Plan as Appendix A.

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11 .O WASTE STREAM MANAGEMENT

Recycle to the process Compact to volume reduce Packaged empties in drums Neutralize/Stabilize/C ompact

Cement stabilization processing produces minimal quantities and types of secondary waste. The only process waste produced is waste water, which is recycled back to the cement process. The other secondary wastes produced as a result of bench scale and pilot scale testing are Personnel Protective Equipment (PPE), empty bulk reagent containers, and lab reagents and lab equipment.

N/A

Sanitary Landfill

RCRA Facility

ZCRA Facility

1 1 .1 Regulatory Issues Specific to Testing Facility

PPE, Fill head Baas

With proper segregation and good housekeeping practices, the secondary waste generated should be potentially contaminated with only the regulated constituents in the surrogate formula. The secondary wastes will be packaged and transported for disposition to a RCRA TSD facility or applicable landfill. The table below summarizes the projected secondary waste generation and management approach.

1-2 cu. ft.

Waste Stream I Volume

I 21000 Gal1ons Waste Water

Treatment Method I D i s DOS %on

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12.0 REPORTS

12.1 Weekly Teleconferences

During the Proof of Principle Testing, CNS will participate in weekly telephone conferences with FDF project personnel and will provide status and progress. Additional telephone conferences will be conducted if testing activities require. Telephone conversation logs detailing subjects discussed will be completed and included as an attachment to the final report. The weekly reports shall reflect the issues discussed during the teleconferences. Weekly teleconferences are to take place every Tuesday at 1 :00 PM EST for the length of the project.

12.2 Weekly Written Reports

During the Proof of Principle Testing, CNS will keep FDF informed of the progress through one to three-page weekly reports. Weekly reports are to be submitted to FDF every Monday by 4:OO PM EST via fax or e-mail, and to contain, as a minimum, the following items:

0 Safety Issues 0 Activities 0 Results 0 Schedule 0 Status of Project Relative to the Work Plan

Issues 0 Plans for the Next Two Weeks 0 Action Item List 0 Conference Call Minutes from the Previous Weekly Teleconference

12.3 Final Report

The draft of the final report will be submitted for FDF review and concurrence. The report will include the following:

0

0

0

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Description of testing; Results of testing runs, including failures; Downtime durations and causes, and corrective actions; ChemicaVphysical data to charaderize the untreakd surrogate slurries and treated residue; Results of preliminary lab test; Conditions of experiments; I

Information on the projected use of filters, types and number of filters, their history in similar applications and potential technical challenges they might present. Observations;

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Volume of treated surrogate produced; Volume of secondary waste produced and requiring treatment; Samples collected, conditions, and analytical data packages, log books; Logs and worksheets Interpretation of the results; The prescribed recipes/formulas with recommended allowable constituent variation; Graphs showing interrelated key parameters; Safety issues associated with the process; Challenges associated with scale up to the full-scale remediation facility ; Implementation; Schedule elements for the full-scale remediation facility; Cost elements for the full-scale remediation facility; and Conclusion.

In discussing the above topics, product performance will control waste loading and waste loading will determine amount of final waste form. The volume of final waste form and perhaps weight will determine cost of raw materials, operational time, maintenance, storage, shipping and disposal costs. Waste loading will have minor impact on plant design.

In the proof of principle testing, CNS does not plan to break waste loading down into small increments such as 50 wt %, 49 wt %, 48 wt %, etc. Laboratory testing will determine an optimum mix design that maximizes waste loading and meets product performance requirements as defined in the RFP and discussed in CNS’s proposal and draft work plan. This defined waste loading will be acceptable within the analytical limit of error for RCRA metals.

Proof of Principle testing is being performed on a well defined surrogate waste. This surrogate waste stream will be certified prior to waste form preparation and testing. Based on such a waste stream, only waste forms containing maximum loading, based on laboratory tests, will be produced.

The main drivers are lead(regu1atory) and sulfate(product quality). The lead w-ill be rendered insoluble by that addition of a predetermined amount of phosphate. Sulfate will be manageu by the selection of a low alumina cement and the addition of a high quality ASTM class F fly ash to produce a less permeable product. It should be noted that barium, lead, and calcium sulfates are relatively insoluble under controlled pH conditions. Fly ash helps in maintaining a lower(c12.5) pH by reacting with available lime. Chromium will be reduced to Cr(lll) prior to precipitation. Other characteristically hazardous metals will be precipitated as the sulfide. Excess sulfide will be managed by the addition of ferrous sulfate. Amounts and order of chemical additives will be determined in lab scale testing. Verification will be accomplished during pilot scale

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4

L’

testing. Formula, chemical additives and addition sequence will be verified during pilot scale testing.

Cost of materials will be discussed in unit amounts and total cost. Costs will be based on amount of materials used and time required to addlprepare materials for use in the process.

CNS plans to use the same size equipment in the POP operation that will be used in full scale operations. The headers which has the equipment for the addition of waste stream , stabilization materials and de-watering fits on to the liner(i.e. mixing drum). All mixing is “in-drum”. Most chemical additives, or perhaps all, will be added to the waste staging tank prior to transfer to the mixer.(liner). The way the CNS system is designed, larger does not represent faster out put. To increase production rates, another header station is added. This serves several purposes: (1)fulI production is not lost due to equipment failure and scheduled maintenance. (2)Permits staging another mix as one is being mixed and moved to the curing and holding area.

During the POP, CNS will determine the amount of time it takes to stage a tank. It is expected that chemical additives will be added to the staging tank and well mixed prior to transfer to the mixing container (liner). The time required to make transfers, add materials, mix, remove header, move to curing room and decontamination of outer surface will be measured. Curing time and final closure will be determined both in time lapsed and labor hours required to perform the operation. It is expected that the process flow will result in a staggered operation which efficiently utilizes equipment and operations personnel.

CNS is aware of the unique nature of the radioactive content of silo 1 and 2 residues. Much of CNS’s experience is with nuclear utilities waste that requires shielding for gamma radiation. There is much experience within the company on dealing with radon gas. CNS’s partner, Parsons, has worked at the Fernald site for a number of years and is familiar with the radioactive nature of the silo 1 and 2 residues. Parsons has experience in designing radioactive facilities that are remotely operated. Waste Management Nuclear Services(WMNS), parent company of CNS, has a wealth of experience in remote operations, maintenance, the use of protective clothing and operator training.

Discussion will cover shielding for possible neutrons in addition to alpha, beta, and gamma radiation and the management of radon gas.

13.0 SCHEDULE

To accomplish project cost and schedule reporting, Chem-Nuclear will utilize Primavera Project Planner software for collection and reporting of project costs and schedule data.

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13.1 Milestones

Prepare Work Plan and QNQC Plan FDF Review and Comment on Work Plan

and QNQC Plan Address FDF Comments on Work Plan

and QNQC Plan

4 4

3

The table below presents key milestones for the POP project, which were incorporated into the CNS project schedule.

4 8

11

Key Milestones

FDF Review and Comment on Re-

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13.2 Duration

The duration of this project is 48 weeks, as indicated in the table above. Starting day was June 4, 1998, and project completion date will be May 6, 1999. Any changes made to the project duration, FDF must communicate to CNS these changes in writing. In the event CNS find it necessary to change the project duration, it will be CNS's responsibility to get FDF's approval in writing.

13.3 Hold Points

Prior to initiation of the actual POP Testing, CNS will submit and obtain FDF's concurrence on a Work Plan that details the program by which the laboratory and demonstration testing will be conducted and documented. FDF will indicate hold points sessions during the POP Testing during the review process.

13.4 Witnessing Visits

FDF will have the option to conduct witnessing visits, coordinated with CNS, during different phases of the Proof of Principle Testing such as: laboratory and demonstration of process testing; and at any point in the development and testing effort and have independent samples analyzed at an analytical laboratory of their selection with no cost to CNS. FDF will indicate witnessing visits during the POP Testing during the review process.

14.0 MANAGEMENT AND STAFFING

14.1 Project Management

CNWFDF interface, division of authority/ responsibility for POP Testing will be the following:

Project Sponsor

Responsible for oversight, establishing project organization, priority setting, conflict resolution and ensuring project objectives support CNS strategic plans. The project sponsor is Pat Hopper

Project Manager

The Project Manager will be responsible for overall project direction including resource allocation, scheduling, integration, and reporting. The Project Manager will be FDF's point for all matters concerning CNS's performance including contractual matters, health and safety issues, operational problems to name a few. He will maintain oversight of CNS activities on the project without becoming directly involved with routine day to day operations. The Project Manager for this project is Kelly McCuny.

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Health and Safety Supervisor

The Health and Safety Supervisor will be responsible for all hazardous aspects of operations. He will also be responsible for insuring that possession limits of CNS's field license are not exceeded during waste process operations. The Health and Safety Supervisor for this project is Wayne Gaul.

QNQC Supervisor

The Quality Control Supervisor will be responsible for implementing all aspects of the project specific QA plan. The Quality Control Supervisor for this project is Dave Kozlowsky.

Operations Supervisor

The Operations Supervisor will be the lead technician on site and is responsible for the supervision and direction of the demonstration process. The Operations Supervisor for this project is John Lash.

Project Evaluation

Determine the overall project scope, and capabilities and responsibilities of CNS personnel to perform the activities required. Identify key milestones to be met, key personnel for reaching the set milestones, and a project schedule to accomplish the key milestones.

Review project scope to insure that project activities can be accomplished under the conditions/ requirements of CNS's CNCF license.

,

Identify hazards associated with the project and determine general health and safety requirements including control measures, monitoring and training.

Project Development

Identify the project requirements and approach for performing and completion of the project.

Develop the Work Breakdown Structure.

Develop the Organizational Breakdown Structure.

Determine the costs associated with the Work Breakdown Structure and the Organizational Breakdown Structure.

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1869 E- General Methods, Material & EauiDment

CNS's selection of a process method, system design and equipment/ material specifications will take into consideration the following.

8

8

Physical and chemical properties of the waste stream Location of process area Past experience Consequences of spill of release Environmental and Occupational Health and Safety goals

14.2 Staffing

Team members have been selected from the CNS organization such as: Operations, QA, Health Physics, Licensing, Engineering, Finance and Contract Administration. Our technical team includes three of the leading stabilization experts in the U.S. (John Carlson, Jesse Conner, and Earl McDaniel). This cross-functional team will be established under the direction of the Project Manager Kelly McCurry. Mr. McCurry will be assisted by Mr. Ahmad Ghandour, who will be assigned as the Project Controller responsible for tracking scope of work elements, budget and schedule. Figure 3.1 of the Project Specific Safety and Health Plan (PSSHP), attached as Appendix A, is a project specific organization chart that shows the relationship between key positions.

14.3 Training

All personnel involved in this project during laboratory testing, and demonstration process will receive appropriate training as specified in section 5.0 of the (PSSHP). The PSSHP is attached to this Work Plan as Appendix A.

14.4 Documents

This Work Plan and the QA Plan will be approved by FDF to confirm and control the performance of work activities during the implementation of the Contract. Any changes to this Work Plan and the QA Plan will be approved by FDF and CNS prior to their implementation, and will be in accordance with section 2.4.1 of the QA Plan.

In addition, this Work Plan will be followed and updated as necessary to accurately reflect the operations of the Proof G I Principle testing.

The Work Plan and the QA Plan will be controlled through CNS Document Control in accordance with approved procedures, which require formal review of any changes to the document. Quality Assurance audits to ensure compliance with the procedure is an integral part of Document Control and is performed by Quality Assurance personnel.

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15.0 REGULATORY COMPLIANCE

15.1 Licenses

The Proof of Principle Bench Scale Laboratory testing and the 72-hour demonstration will be performed at the Chem-Nuclear Consolidation Facility (CNCF). Although the surrogate waste materials do not contain any radioactive constituents, the facility is operated under the jurisdiction of the State of South Carolina, Department of Health & Environmental Control (SCDHEC) Radioactive Material License 287-04, and this Department shall have ultimate authorization of the POP activities.

15.2 Permits

The Proof of Principle laboratory testing and pilot demonstration is being performed in accordance with the SCDHEC Bureau of Land & Waste Management Division regulations R.61-79, 261.4(e), Treatability Study Samples. The Chem.-Nuclear Consolidation Facility EPA ID Number is SCD987580446.

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(D22498)

APPENDIX A

PROJECT SPECIFIC SAFETY AND HEALTH PLAN

(26 PAGES)

c

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PROJECT SPECIFIC SAFETY AND HEALTH PLAN

(PSSHP)

Silos 1 and 2 Proof of Principle Testing By Chem-Nuclear Systems, LLC

September 29,1998

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TABLE OF CONTENTS u

1 . 0 SUMMARY ......................................................................................................... 3

2.0 I NTRODUCTI ON ................................................................................................ 3

2.2 Facility and Equipment Description ............................................................ 5 2.3 References ................................................................................................. 6

ORGANIZATION AND KEY PERSONNEL ........................................................ 6

3.1 Organization Chart ........................................................................... : ......... 6 3.2 Key Personnel and Responsibilities ........................................................... 7

PROJECT HAZARD ASSESSMENT ................................................................. 8

4.1 Physical Hazards ....................................................................................... 9 4.2 Chemical Hazards .................................................................................... 10

2.1 Project Description ..................................................................................... 3

3.0

4.0

5.0 PERSONNEL TRAINING ................................................................................. 15

6.0 MEDICAL SURVEILLANCE ............................................................................. 16

6.1 Baseline Monitoring .................................................................................. 16 6.2 Periodic Monitoring .................................................................................. 16 6.3 Site-Specific Medical Monitoring .............................................................. 16 6.4 Exposure/lnjury/Medical Support ............................................................. 16 6.5 Exit Physical ............................................................................................. 17 PERSONAL PROTECTIVE EQUIPMENT ........................................................ 17

7.1 PPE Selection ...................................... 1 .................................................... 17 7.2 Protective Clothing ................................................................................... 18 7.3 Reassessment of PPE ............................................................................. 19 7.4 Site Specific Method and Extent of PPE Maintenance and Storage ........ 19 7.5 Site Specific Method and Extent of PPE Decontamination ...................... 19 7.6 PPE Training and Proper Fitting ............................................................... 19 7.7 PPE Donning and Doffing Procedures ..................................................... 19 EXPOSURE MONITORING AND SAMPLING ................................................. 19

7.0

8.0

8.1 8.2 Purpose of Air Monitoring ......................................................................... 20 8.3

9.0 SITE CONTROLS ............................................................................................ 21

Monitoring Requirements for Silos 1&2 Proof of Principle Testing ........... 20

Identifying and QuantifVing Airborne Contaminants ................................. 20

10.0 DECONTAMINATION ...................................................................................... 23

11 . 0 EMERGENCY RESPONSE ............................................................................. 23

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1.0 SUMMARY

2.0

The Project Specific Safety and Health Plan (PSSHP) provides guidance for the proof of principle testing to be conducted at the Chem-Nuclear Consolidation Facility (CNCF). The testing will be conducted in two phases, (1) laboratory (bench) scale testing and (2) pilot scale testing. Each type of testing has been conducted previously at these facilities and the hazards associated with them are well known.

The primary hazard is the potential for airborne hazardous chemicals, which include compounds containing arsenic, chrome, nickel and lead (see Table 2.1 for complete list of chemicals). Airborne dusts will be controlled via three forms of engineering controls; (1) the central HVAC system which is equipped with HEPA filters, (2) local HEPA air movers which can be positioned near the potential source and (3) water mist to wet the powder preventing it from becoming air borne.

Two specific tasks present the most risk for creating an airborne condition; (1) the sieving process that is used to assure particle sizes for the tests and (2) the actual mixing of the chemical components to make the surrogate waste media. These risks are minimized during the laboratory scale tests because of the volume of material involved. Further, a fume hood is available to contain dusts during the sieving task. The sieving and chemical mixing task during the pilot scale testing will require the use of respiratory protection.

Physical hazards to be considered are consistent with an industrial work area. They include pinch points, falling objects, bums, cuts, and muscle strains. These hazards will be controlled using safe work practices, engineering controls and personal protective equipment.

Chemical hazards include the potential exposure to corrosives, oxidizers, absorption, inhalation and ingestion hazards including but not limited to arsenic, lead, chrome, and nickel compounds.

INTRODUCTION

2.1 Proiect DescriDtion

Chem-Nuclear Systems, LLC (CNS), under contract to Fluor Daniel Femald (FDF), will perfohn a “Proof of Principle” demonstration which will provide data to evaluate the use of cement stabilization of certain surrogate waste forms. The surrogate waste forms represent the contents of waste contained in Silos 1 and 2 located at the Femald, OH facility. The project will be completed at Chem-Nuclear Consolidation Facility (CNCF)in Snelling, SC adjacent to Highway 64.

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The project will consist of two phases; (1) laboratory scale testing and (2) pilot scale testing. The laboratory scale testing will result in the development of six recipes for three different surrogate formulas. This information will then be used to refine the mass and energy balances which can be used to develop process flow diagrams (PFDs), specifically in regard to the chemistry involved with the pilot plant phase and subsequent full scale process operations. The second phase, pilot scale testing, will be used to further refine process parameters and calibrate the mass and energy balances.

Sodium Nitrate

Sodium Selenite Vanadium pentoxide Kerosene

Diatomaceous Earth

Lead Carbonate

The surrogate waste forms for both the laboratory scale and pilot scale testing will be prepared at the CNCF following a FDF prescribed formulation. The surrogate waste forms can contain various concentrations of the following chemicals:

NaN03 Nickel Oxide NiO

Na2Se03 Silica Dioxide Si02 v 2 0 5 Zinc Oxide ZnO

PbCO3 Lead Sulfate PbS04

nla Feldspar (Na, K) AIS308 nla

The cement stabilization materials will consist of any or all of the following:

a. Type 1/11 Portland cement b. Organo-phillic material c. Class F fly ash

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d. Additives (if needed)

2.2 Facility and Equipment Description

2.2.1 Lab Scale Testing

The bench scale testing laboratory at the CNCF building 201 consists of standard laboratory bench space and fume hoods. A safety shower is located in the work area.

The following equipment will be utilized for developing cement formulations during the laboratory scale testing:

a. b.

d. e. f. 9- h. I.

k.

C.

j.

Electronic balance Hobart mixer Compression tester Pocket penetrometer pH meter Brass molds Disposable molds Various laboratory glassware Spatulas Curing (oven) cabinet Plastic wrap or Parafilm, zip-lock bags

2.2.2 Pilot Scale Testing

The pilot scale testing will occupy a 4,0OOf? footprint in the main CNCF building 201 operating area. This area is adjacent to a radiation area and may be considered a “radiation controlled area”. It is serviced by a HVAC system with a HEPA filtered exhaust.

The following equipment will be utilized during the pilot scale testing:

a. b.

d. e. f. 9- h.

C.

I.

j. k.

Drum conveyor system Local HEPA filtered air movers Media auger Process fillhead and support equipment 85 gallon drums Surrogate waste mixing containers Mixer head Dewatering containers Positive displacement pumps Mixing blades Temperature Monitors

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,

_______________________________

I I

*- 1869

QA /QC - Dave I Kozlowsky

I. Air samplers m. Overhead crane n. Forklift (if necessary)

r

SHO Treatability Pilot B. Well Mgr. ’ Operations

R. Dabolt J. Lash

2.3 References

Spl. 8l

Analysis N. Frink

2.3.1 29 CFR 1910.120, “Hazardous \ Response”

laste Operations and Emergency

2.3.2 29 CFR 1910.1025, “Lead Standard” 2.3.3 29 CFR 191 0.1 01 8, “Arsenic Standard” 2.3.4 29 CFR 1910.1000, “Air Contaminants”, Table Z 2.3.5 29 CFR 191 0.1200, “Hazard Communication” 2.3.6 CNS Procedure, DF-SF-009, “CNCF Health And Safety Program” 2.3.7 CNS Procedure, CN-EM-001 ,- “Emergency Response” 2.3.8 NlOSH Pocket Guide to Chemical Hazards, June 1997

3.0 ORGANIZATION AND KEY PERSONNEL

3.1 Organization Chart

Figure 3.1 is a project specific organization chart that shows the relationship between key positions.

PROJECT ORGANIZATION Figure 3.1

FDF Technical

Representati

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3.2 Kev Personnel and ResDonsibilities

3.2.1 Project Manager - Kelly McCurry

0 Management of the project; Confirmation of each team member s suitability for work; based on person’s training and physical condition;

0 Briefing the team on their specific assignments; 0 Coordinating with the SHO on safety and health requirements; 0 Assuring proper records are maintained; 0 Preparation and submittal of required reports; and

Liaison with FDF Technical Representative.

3.2.2 Treatability Manager - Rich Dabolt

Execute the work plan; 0 Supervise formulation development;

Develop treatability Proof Of Principle Plan (POP); Implement project-specific QA & ES&H procedures; and

0 Coordinating with the SHO in determining appropriate PPE.

3.2.3 Pilot Operations Manager - John Lash

Manage pilot scale tests; 0 Execute the work plan; 0 Enforce site control; 0 Document test activities; 0 Coordinate with the SHO in determining appropriate PPE; 0 Developing, implementing, and updating the emergency

response/emergency action plan, as necessary to reflect conditions; and

0 Assuring the evacuation, emergency treatment, emergency transport of site personnel and notifying emergency response units and management.

3.2.4 Sampling and Analysis Manager - Neal Frink

0 Develop and implement a Sampling and Analysis Plan; 0 Data collection and management;

Monitor environmental emissions; 0 Coordinate with the SHO in determining appropriate PPE.

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3.2.5 Project Controls Manager - Ahmad Ghandour

0 Tracks schedule; Tracks budget;

0 Initiates project activities; and 0 Provides verbal and written status reports to the Project

Manager.

3.2.6 Environmental, Safety and Health Manager - Wayne Gaul

0 Supervises the SHO's activities; 0

0

0

Provides technical support to the project;

Addresses ES&H issues pertinent to the project; Assesses safety and health issues pertinent to the project; and Reviews and approves project specific plans and procedures.

3.2.7 Safety and Health Officer - Brad Well

0 Implements the Project Specific Safety and Health Plan (PSSHP);

0 Assures safety measures are properly taken during the project;

0 Reports unsafe conditions to the Project Manager; 0 Issues stop work order if unsafe condition could result in

severe injury or death; and 0 Coordinates SHO activities with CNS Health Physics

personnel.

3.2.8 QNQC Manager - Dave Kozlowsky

0 Review, verify, and approve records; 0 Identify, report, track, and approve requirements for

nonconforming systemskomponents; 0 Verify requirements for systems, structures, and components;

and 0 Inspections and tests required for the project.

4.0 PROJECT HAZARD ASSESSMENT

A hazard assessment for the Proof of Principle project has been completed. The assessment evaluated both physical and chemical hazards.

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4.1 Physical Hazards

Handling chemicals and drums by hand

This project will not involve any confined space or extreme temperature hazards. The work will be conducted in the temperature-controlled environment of the laboratory and operating areas of Building 201. The general physical hazards include the risk of falling objects, slipping and tripping hazards, pinch point hazards, cuts and abrasions, and bums.

1. Muscle sprains. 2. Foot injuries 3. Hand injuries 4. Eye injuries 5. Head injuries

1

Each step of the Work Plan was evaluated to determine the specific hazards associated with it. Identified hazards were then evaluated to determine the best means of mitigating the hazard. CNS's po!icy is to use engineering controls, if possible, as the first means of mitigation. Engineering controls are supplemented with administrative controls including safe work practices and, if necessary, personal protective equipment. Table 4.1 provides a more detailed evaluation of the physical hazards and means of mitigation for each major task.

Developing formulations

PHYSICAL HAZARD ASSEMENT

Table 4.1

1. Hand injuries 2. Eye injuries

I TASK I HAZARD

shields will be worn.

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1869 Tu--

TASK HAZARD

4.2

CONTROLS

3. Work areas will be maintained in a clean condition.

4. Slip and trip hazards will be corrected upon identification.

Chemical Hazards

An evaluation of each of the chemicals used to make up the surrogate waste was completed. The NIOSH “Pocket Guide To Chemical Hazards”, June 1997 addition, OSHA’s PEL’S found in Table A of 29 CFR 1926.1450, specific OSHA Standards (29 CFR 1910.1025,29 CFR 1910.1018, and 29 CFR 1910.1000), and the applicable Material Safety Data Sheets (MSDS) (see Appendix A).

The primary chemical hazards will be associated with the use of lead, chrome, nickel and arsenic containing compounds. Another potential hazard is the possibility of generating airborne dust during the sieving of silica containing compounds. To mitigate these hazards CNS proposes to use two types of engineering controls, local HEPA air movers and water mist. In addition, the use of stay time controls and personal protective equipment including respiratory protection will be used to supplement the engineering controls. Under normal operating conditions neither the PELs nor action limits established by OSHA are expected to be exceeded.

Table 4.2 summarizes information for each chemical found in the surrogate waste. The primary source of information was the Material Safety Data Sheet for the specific compound. The NIOSH Pocket Guide was used for supplemental information and to verify the MSDS. The MSDSs for chemicals being used to make up the surrogate waste can be found in Appendix A. Please refer to the MSDSs or NIOSH Pocket Guide (reference 2.3.8) for information regarding specific chemicals, including routes of entry, PELs, symptoms of exposure, and first aid.

Several of the chemical compounds including those containing arsenic, chrome, lead, and nickA are toxic. Their primary route of entry is inhalation with ingestion being a secondary route of entry. The target organs include the blood forming organs, central newous system, respiratory system, kidneys and. liver.

Tributyl phosphate is corrosive and can be absorbed through the skin. Persons exposed to this material should wash the area with soap and water.

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,

Persons who have had an inhalation exposure to any of the chemicals found in Table 4.2 should be removed to fresh air. If respiratory problems develop be prepared to assist victim. Transport to medical facilities as soon as practical if respiratory distress is noted.

Persons who have had an ingestion exposure to any of the chemicals found in Table 4.2 should be transported to medical facilities for further evaluation and treatment.

If exposure consists of skin or eye contact, the affected area should be flushed with copious amounts of water for a minimum of fifteen minutes. Skin areas may be washed using a mild detergent to assist in removing insoluble material. If skin rash develops seek medical assistance. All eye contact should be followed up with an medical evaluation.

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40-Hour HAZWOPER

8-Hour Sup IMgr.

HAZWOPER

c 1869 'L,

Project Controls Manager

X

X

5.0 PERSONNEL TRAINING

Pilot Operations Manager

X

X

The initial training provided shall be applicable to the industrial and occupational hazards and regulatory requirements associated with this project. Personnel shall have received 40-hour HAZWOPER training in accordance with 29 CFR 191 0.1 20 or an 8-hour refresher class for employees that have previously had the 40-hour HAZWOPER training. All supervisors shall have received an additional 8-hour HAZWOPER supervisor-training course. Practical demonstrations shall be given, when appropriate. The training shall be commensurate with the anticipated work hazard and will include discussions of the Proof of Principle Testing, industrial safety, and emergency procedures. Subcontractors will furnish copies of their training certificates or supply company letters stating worker-training qualifications. Copies of training records shall be accessible to the SHO

5.1 Specific Requirements

The following training is required of all personnel on this project:

ES&H Safety & QAlQC First Aid Techni Manager Health Inspector Providers cians

Officer

X X X X X

X X X X X

PROJECT TRAINING MATRIX

8 hour HAZWOPER

update 24-Hour

Supervised Field

Experience Respiratory Protection Lead Std.

Inorg. Arsenic Std.

First Aid

LockoutlTagout

X

X

X X

' x

X

X X

X

X Hazard Communication Confined Space

Fire Extin uisher

CPR

X X X X X

X X X X

X X X X X X X X X X

X X X X X X X X

X X X X X X

X

~

x X X X X

X X X X X X X

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1 Blood borne

ES&H Manager

l-

Safety & QAlQC First Aid Techni Health Inspector Providers cians Officer

(Project specific)

X

X X I X

X X X X

X X X X

6.0 MEDICAL SURVEILLANCE

6.1

6.2

6.3

6.4

Baseline Monitoring

Prior to being assigned to a hazardous or a potentially hazardous activity involving exposure to hazardous materials, each employee must receive a baseline physical. At a minimum, the following medical tests will be performed:

Complete medical and work histories. Physical examination. Pulmonary function tests (FVC and FEW). Chest X-ray (physician’s option) EKG (physician’s option) Eye examination and visual acuity. Audiometry. Urinalysis.

Periodic Monitorinq

In addition to a baseline physical, all employees require a periodic physical within the last 12 months unless the advising physician believes a shorter interval is appropriate.

Site-SDecific Medical Monitorinq

As determined by the SHO and ESH Manager, workers will provide barsline and exit biological sample. (blood, urine, and/or fecal) if exposure to hazardous materials warrants such samples.

Ex~osu re/l n iu rv/M ed ical S u D D O ~

As a follow-up to an injury or possible exposure above established exposure limits, all employees are entitled to and required to seek medical attention and physical testing. Depending upon the type of exposure, it is

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critical to perform follow-up testing within 24-48 hours. It will be up to the CNS’s medical consultant to advise the type of test required to accurately monitor for exposure effects. The ESH Manager will be notified of personnel injuries, safety-related incidents and exposures. Individuals receiving exposures over the Permissible Exposure Limits (PEL’S) of contaminants or agents to which they are exposed or are injured will be referred immediately to a local physician for treatment.

6.5 Exit Phvsical

At termination of employment or reassignment to an activity or location, which does not represent a risk of exposure to hazardous substances, an employee will complete and exit physical. If hidher last physical was completed within the last 6 months, the advising medical consultant has the authority to determine the adequacy and necessity of an exit exam.

7.0 PERSONAL PROTECTIVE EQUIPMENT

As stated in 29 CFR 1910.120(b)(4)(ii)(C), the SSHP specifies what personal protective equipment (PPE) is to be used by employees for each of the site tasks and operations being conducted in accordance with 29 CFR 191 0.1 20(9)(5). The information in this section comprises the written PPE program for the project.

7.1 PPE Selection

The following is a summary of the PPE that will be used for the Silos 1 & 2 Proof of Principle Testing.

0 Any employee or visitor who enters the work area and is not in a break area must wear at least Level D PPE. Level D PPE consists of hard hat, safety eyeglasses, and steel-toed work boots. Any exception to this must be approved in advance by the ES&H Manager.

0 Any employee or visitor who enters a contaminated area must wear Level D PPE and anti-contamination garments (PCs or Anti-Cs) as required by the SHO. An Air Purifying Respirator (APR) with HEPA filter cartridges shall be used when entering an airborne contamination area as directed by the SHO.

Anti-C Garments include the following;

TyVekTM Coveralls (or equivalent) 0 TyVekTM Hood (or equivalent, may be attached to coveralls)

BootCovers 0 Rubber Gloves (or as specified by the SHO) 0 Air Purifying Respirator with HEPA Cartridge (as required by the SHO)

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The following table details the minimum PPE required to perform each task during the project.

Developing formulations.

PPE Requirements by Task Table 7.1

WorkGloves LabCoat Safety Glasses Rubber Gloves Work Gloves (when handling items from oven and when handling broken glass)

TASK PPE Sieving dry powders in bulk.

Mixing dry powders in bulk.

Boot Covers Rubber Gloves

0 Air Purifying Respirator with HEPA cartridae

Safety Shoes Coveralls Hood Boot Covers Rubber Gloves Air Purifying Respirator with HEPA cartridge Safety Shoes Safety Glasses

7.2 Protective Clothinq

CNS shall require anti-C coveralls for protection against contamination. Appropriate rubber gloves and boot covers are to be worn over hands and work boots where potential hazardous conditions are applicable. Boots shall have steel toes. Hard hats and safety eyewear are routinely required.

Protective clothing requirements for all contaminants shall be identified by the SHO, who shall put this in writing to convey requirements to personnel. A pre-job brief stressing PPE requirements shall be conducted

:: prior to proceeding with work.

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7.3 Reassessment of PPE

The level of protection provided by PPE selection shall be upgraded or downgraded based upon a change in site conditions or findings of investigations. The SHO will contact the ES&H Manager prior to any upgrades or downgrades in level of protection or monitoring frequency. When a significant change occurs, the hazards should be reassessed. Some indicators of the need to reassess are:

Change in job tasks during work phase. 0 When individual medical considerations limit the effectiveness of PPE. 0 Other contaminants are encountered. 0 Change in levels of contaminants in the work area. 0 Change in the degree of contact with contaminants.

7.4 Site Specific Method and Extent of PPE Maintenance and Storaqe

CNS will be responsible for maintaining inventories of PPE as required by operations; however, each employee is responsible for inspecting hidher own PPE before donning. Inspection will consist of: 1) inspecting for holes in garments; 2) functions as intended; 3) fits properly; 4) proper selection as specified by the SHO.

7.5 Site Specific Method and Extent of PPE Decontamination

The SHO shall list the tasks and specified levels of protection required for each job. Consistent with the levels bf protection required, the SHO will provide personnel decontamination capabilities.

7.6 PPE Traininq and Proper Fittinq

Covered and documented during the Pre-Job Briefing and 40-hour HAZWOPER training in accordance with 29 CFR 1910.120(e).

7.7 PPE Donnina and Doffinq Procedures

Donning and doffing of PPE will be covered during the Pre-Job Briefing and 40-hour HAZWOPER training. Detailed instructions are contained in CNS work procedures.

8.0 EXPOSURE MONITORING AND SAMPLING

This section explains the general concepts of the monitoring program by CNS. The following table shows the types of sampling by location.

(4 -3

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8.1 Monitorina Reauirements for Silos 1 &2 Proof of Principle Testinq

Air Monitoring Type & Frequency Table 8.1

Sample Type 1 Sample Frequency I Air Monitoring One sample will be drawn during 0 8-hour TWA for nickel, lead, the preparation of surrogate waste

arsenic and chrome collected on a for the Pilot Scale Test. A second glass fiber filter paper with a sample will be drawn as personal lapel samDler’. necessary.

Noise Levels With decibel meter

Initially during mixing operations.

8.2

8.3

Heat Stress (physiological indices) Only required if work is performed outside of climate controlled atmosphere. Frequency will be determined by SHO

Purpose of Air Monitorinq

The purpose of air monitoring is to identify and quantify airborne contaminants to determine ambient concentrations and the level of worker protection needed. Initial screening for identification is often qualitative, i.e., the contaminant, or the class to which it belongs, is demonstrated to be present but the determination of its concentration must await subsequent testing. Exposure monitoring results shall be provided to the ES&H Manager for review and to the employee being monitored, as appropriate.

ldentifvina and Quantifvina Airborne Contaminants

Laboratory analysis of air samples obtained by gas sampling bag, collection media (Le., filter, absorbent) and/or wet-contaminant collection methods will be utilized at the direction of the SHO.

The analytical results of the air sample will be used to develop scaling factors for those compounds other than containing arsenic, chrome, lead and nickel.

1

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9.0 SITE CONTROLS

9.1 Site Access

Access to the CNCF Building 20l(see Figure 9.1) will be controlled in accordance with the CNS security program. A security fence surrounds the building and access to the building is controlled. Only trained personnel have access to the building. Access to the laboratory and operating areas is further controlled and limited to personnel having specialized training. Visitors must be escorted at all times.

9.2 The lab scale tests will be run in the laboratory area. This area is equipped with fume hoods and standard laboratory equipment. Access to the area during testing will be limited to those persons specifically responsible for these tests.

9.3 The pilot scale tests will be run in an area of the main operations area of the building. The contamination and exclusion zones will be designated by appropriate barrier. Work in the exclusion zone will be accomplished using the "Buddy System" where a minimum of two people must be in the area at a time when work is on going (excluding safety, industrial hygiene, and rad control activities). At least one person shall be located in the Support Zone adjacent to the exclusion zone when testing is being done.

9.4 Local HEPA air movers and water spray will be used to minimize dust release when sieving or mixing. If these controls are insufficient, personnel in the exclusion zone will be required to wear respiratory protection when these activities are being done.

9.5 Existing CNCF and CNS, and/or project specific procedures shall be used to control work activities.

9.6 Medical assistance is available locally from trained first aid/CPR providers. Injuries requiring additional medical treatment will require transportation to the local Bamwell County Hospital (See Emergency Response section).

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.

Chem-Nuclear Consolidation Facility Partial Floor Plan

For Proof of Principle Tests

Figure 9.1

\ Main

1 Locker Room

Women's Locker Room

- 7 Exit/Entrance La borato

Stairs to 2 Level Support Zone

'Safety Shower

I I I

I Safety 9 Shower

Pilot Scale Test

%Emergency I Exit

d--Truck Bay Door

CNCF Waste Processing Area

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.

10.0 DECONTAMINATION

\

Personnel decontamination requirements shall be minimal under normal conditions. Potential contamination shall be controlled by local HEPA air movers and water spray to prevent airborne dusts. In addition, chemical additions and mixing is accomplished under semi-remote conditions limited operator access to the potentially hazardous materials.

10.1 Persons leaving the exclusion zone will doff the outer layer of chemical protective clothing while moving into the decontamination zone.

10.2 All persons leaving the decontamination zone will proceed to the shower area and remove remaining protective clothing. These people will be required to complete a full body shower before exiting the shower area.

10.3 All tools and equipment used in the exclusion zone will be decontaminated or properly contained for disposal prior to leaving the controlled area. Decontamination shall consist of a minimum of three water rinses and manual wipe down.

11 .O EMERGENCY RESPONSE

11.1 Personnel assigned to this project will take appropriate action to contain small spills and to extinguish fires in the incipient phase. All other emergencies will be handled in accordance with the CNS Procedure for Emergency Response, CN-EM-001.

11.2 Medical emergencies shall be reported to the CNCF facility manager, or designee, immediately.

11.3 The emergency numbers applicable to this plan are listed below:

NAME AND TITLE Work Phone No. Home Phone No.

Kelly McCurry - Project Manager

Wayne Gaul - ES&H Manager

758-1 848

259-5036

Brad Well - Safety and Health Manager 654-1 353 pager

Lynne Garner - Treatability Manager 259-5068

803-732-9355

John Lash - Pilot Operations Manager and Facility Manager

259-5067

~

CNS Security

Barnwell County Hospital

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11.4 In case of an emergency the route to the local hospital is shown in Figure 11.1.

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MAP DEPICTING ROUTE TO BARNWELL COUNTY HOSPITAL

Figure 11.1

CNCF b

REYNOLDS RD -

AIKEN BY - PASS

I ENTRANCE SRS 1

HWY 64 \

H W Y 6 4 .-bl I

1 HWY 278

COUNTY H 0 SPITAL

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1

(D22498)

APPENDIX B

MATERIAL SAFETY DATA SHEETS

(PROVIDED UPON REQUEST)

b

PL-CNSI-98-004 REV. 0 PAGE 88