New 7693 Autosampler and Multimode Inlet for

Easier Methods Development and Improved GC and GC/MSand Multimode Inlet for

Drinking Water Analysisand Improved GC and GC/MS Sensitivity

Mike SzelewskiAgilent TechnologiesWilmington,DEApril 22, 2009April 22, 2009

If you could…

Run more samples in your sequence

Improve detection limits

Automate tedious sample and standard preparation steps

Handle active compounds better than beforep

Make large volume injections without spending a long time on method development

Get better precision

…wouldn’t you be happy!

Two New Products from Agilent to Enhance Lab ProductivityProductivity

Agilent 7693A Automatic SamplerAgilent Multimode

Agilent 7693A Automatic Sampler Inlet

New 7693A Automatic Liquid Sampling System

New Tray with 150 Vi l P iti

New Injector with 16 Vi l P iti

Page 4

Vial PositionsVial Positions

7693A Injector & Tray Features• 16 (Injector) and 150 (Tray) , 2mL samples• Removable, 50 vial sample trays• Injections from 1-50% of syringe size in

Setting (injecting into S/SL inlet)

Precision (%RSD)

20% to 50% 0 30%j % y g1% increments

• Modular, field repairable • Self Calibrating, alignment like 7683B

20% to 50% 0.30%10% 0.80%2% 1-2%1% 3-5%Self Calibrating, alignment like 7683B

• LVI (Large Volume Injection to 250µl per injection)• Single Sample Heater, Barcode reader/ mixer• Active gripperActive gripper• Compatible with all 6890, 7890, 7820 and 6850

(Injector Only)• Optional heater/chiller plate (requires circulating bath)p p ( q g )

Removable 50 Vial Sample Tray for 2 ml Samples

New 16 Sample Capacity in ALS Injector

7673C 7683B 7693A

Page 7

Sandwich Injections with 7693A

• Sandwich Injections are possible with single tower• Air gaps are optional

• Lifetime before failure 120 000 injections

Lifetime and Reliability Testing• Lifetime before failure – 120,000 injections

Sample Prep Programming Flexibility

Sandwich injections ( up to 3 layers with air gap)• Examples of Simple liquid manipulation

• ISTD addition• ISTD addition• Reconstitution• Mixing (Requires Bar Code Reader / Heater/ Mixer option)• Dilution• Derivatization• In Vial Extraction• In Vial Extraction

Ambient In-vial Small-Volume Derivitization Dilution Internal Standard Heating/MixingH d E t ti S li Additi B C dHeadspace Extraction Sampling Addition Bar Code

Example Sample Prep Method for Preparing StandardsStandardsPrepare 7 levels of standards, plus a blank

Add varying amount of solvent to vials with inserts (270 – 300 uL )Add varying amount of solvent to vials with inserts (270 300 uL )

• Use a wash bottle as a solvent source in rear towerAdd varying amount of standards to 7 vials ( 30 – 0.3 uL)

• Stock standards solution in a front turret positionAdd fixed amount of ISTD solution to 8 vials ( 3 uL)

• Stock ISTD solution in a front turret position

Total 100 steps 50 minutes plus 10 minutes setupTotal 100 steps – 50 minutes plus 10 minutes setup

Compare Manual prep vs 7693A prep, Ratio of%RSDs of RRFs from 7 level cal%RSDs of RRFs from 7 level cal

1 6

1.8

2

nua

0.8

1

1.2

1.4

1.6

omat

ed /

%R

SD M

a

0

0.2

0.4

0.6

0 8

0 - e s e e e l l n e 0 n T 2 e e e 2 n n

%R

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uto

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7693A is as good as a skilled chemist when making a 7-level calibration set

New Multimode Inlet for Gas Chromatography

Current Agilent PTV – Support IssuesNeedle bindingPlugged split line Needle binding

Leaks at liner

Plugged split line

Broken liner

Only cryogenic cooling

Small liner volume

g

Stripped threads

Page 18

Agilent’s New Programmable Inlet - MMI

7890 turn-top

7890 standard pneumatics Uses 7890 S/SL

liners, septa and , po-rings

Air plus CO2, N2 cryogenic cooling

7890 t d d

cryogenic coolingThermocouplesensing

7890 standard capillary fitting

Agilent Multimode Inlet Features HardwareHardwareTemperature range of -160ºC to 450ºC

Heating @ 15ºC/sec

Septum/Liner Easily Changeable

Injection Modes: Hot S/SL, Cold S/SL, PTV in pulsed mode, solvent vent mode, residue removal mode

Support for single stroke injections from 0.1 μL to 250 μL

EPC Compatible with Packed Liners

Compatible with 7890A 5975C 7683A/B CTC Combi PALCompatible with 7890A, 5975C, 7683A/B, CTC Combi PAL

SoftwareTen temperature ramps

Solution for solvent vent timing

Integrated into ChemStation, MSD ChemStation, EZChrom, MassHunter

MMI Programmable Temperature Vaporizing Inlet – injection modesVaporizing Inlet injection modes

Hot split/splitless (also pulsed)similar to the S/SL inlet using the same liners• similar to the S/SL inlet using the same liners

Cold split/splitless (also pulsed)• Significantly more inert than hot splitlessSignificantly more inert than hot splitless• Can inject 3-5 uL with no solvent venting• Better sensitivity than hot splitless because large vapor cloud

is not formed which travels outside the liner and portions areis not formed which travels outside the liner and portions are lost

LVI-Solvent Vent• An extension of cold splitless• Large volume injection for maximum sensitivity

Multiple Mode GC Inlet - Cold Injections

• No syringe-needle discrimination; Minimal inlet discrimination

N i l i li bl• No special syringes, liners or consumables

• Large volume injection (5ul to 250ul) - lower detection limits

• Solvent vent/matrix vent decrease interference / maintenance• Solvent vent/matrix vent - decrease interference / maintenance

• Flexibility (hot/cold split/splitless, temperature programmed vaporization)

• Cold trapping in liner - improves chromatographic peak shape, resolutionCold trapping in liner improves chromatographic peak shape, resolution

• Capillary column backflush with CFT - decreases cycle time, maintenance

MMI Cold Splitless and SV – Temperatureand Flow Programsand Flow Programs

Transfer of sample from inlet to column GC Separation

Cold Injection

MMI Temp 20 350

MMI cooldown

0.9 min

MMI Temp

GC Oven Oven = 40Oven ramps

20 350

GC OvenTemp

P

Oven = 40

PurgeStatus purge off purge on

0 0.05 2.5 26Min 1.50.6

Multimode Injection of Triazine Herbicides

1µL Cold Splitless injection

1µL Hot Splitless injection

5.52 5.54 5.56 5.58 5.60 5.62 5.64 5.66 5.68 5.70 5.72 5.74 5.76 5.78 5.80

1, 2, 3 and 4 µL Cold splitless injections (ethyl acetate)

5.55 5.60 5.65 5.70 5.75 5.80 5.85 5.90 5.95 6.00 6.05 6.10 6.15 6.20 6.25

Compare cold to hot splitless S/N using the new Multimode Inlet on a 7890-5975 GC/MSD systemMultimode Inlet on a 7890 5975 GC/MSD system

RatioRT Mass Cold S/N :

Hot S/N

Fluorene 11.152 166 1.36Most “active”Aldrin 15.205 66 1.33

263 1.33compoundgives largestimprovement Mevinphos 9.338 127 1.33

Pentachlorophenol 12.989 266 2.19

improvement

Endrin 17.600 263 1.48

p,p'-DDT 18.600 235 1.51

Area Ratios of 1-5 uL Cold SL to 1 uL Hot SL using the New MMI, single taper helix linerthe New MMI, single taper helix liner

Normalized hot splitless area = 1Normalized hot splitless area = 1

Compare hot-to-cold splitless %RSDs using the new MMI on a 7890-5975 GC/MSD system, 7 level cal

PTV - Solvent Vent (elimination) Mode

Set inlet temperature at or B ffl d

Syringeneedle

pbelow solvent boiling point

Set high split ratio

BaffledLiner

Carrier

Inject sample very slowlyinto PTV

Solvent evaporates through

Vent

p gsplit vent

Close split vent and rampPTV temperature

SampleAnalyteSolvent p

Carry out separation onanalytical column

Column

MMI Cold Splitless and SV – Temperatureand Flow Programsand Flow Programs

Transfer of sample from inlet to column GC Separation

Cold Injection

MMI Temp 20 350

MMI cooldown

0.9 min

MMI Temp

GC Oven Oven = 40Oven ramps

20 350

GC OvenTemp

P

Oven = 40

PurgeStatus purge off purge on

0 0.05 2.5 26Min 1.50.6

New Multimode Inlet “Solvent Elimination Wizard” Built-into ChemStation for Easy Method Development

Solvent Elimination Calculation Wizard

Step 1Step 1

Time for Optimal Solvent Elimination Relates to Temperature, Pressure, Flow, Type and VolumeTemperature, Pressure, Flow, Type and Volume

St 2Step 2

Upload Parameters to your Method

Step 3Step 3

All inlet &injection parameters determined for youdetermined for you

25 Pesticide Standards at 40 ppb in Acetone(plotted on the same scale)

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in

25 µL Solvent Vent (35C)n I

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10-µL Cold Splitless (30C)

2-µL Hot Splitless (280C)

10-µL Cold Splitless (30C)

4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00

µ p ( )

Compare Hot SL, Cold SL and SV - %RSDs of 7 Level Cal using the new MMI on a 7890-5975 GC/MSD system

60.0

70.0

40.0

50.0

1uL HSL

3uL CSL

10 0

20.0

30.0 25uL SV

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10.0

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SL=100-10,000 ppb, SV=1-100 ppb

MMI LVI-SV, Save Time and money with Reduced Sample Prepwith Reduced Sample Prep

Assume the concentration of a water sample is 1ng/mL

Concentrate before inj …• Sample Volume = 1000 mL

Use LVI instead …• Sample Volume = 100 mL

• Extract 1000 mL and reduce to 1 mLConc = 1000 ng/mL

• Extract 100 mL and reduce to 1 mLConc = 100 ng/mL

• Inject 1 uL into the GCAmount injected = 1 ng

• Inject 100 uL into GCAmt injected = 10 ng

New MMI-LVI Methods DevelopmentWhere do I start ?Where do I start ?

Much easier to develop methods with the new inlet –liner, column and starting conditions remain intact !, g• 1 ul injection of your standard in splitless mode• 3-5 uL injection in cold splitless – stop here if good sensitivity• 5 ul injection in solvent vent mode• 25 ul injection in solvent vent mode• Move up in volume from here if necessary• Move up in volume from here if necessary

Always use an empty vial as a test for LVI single or multiple injections

Agilent's New GC Products

• Agilent's New 7693A ALS increases sample throughput– Auto-alignment, easy installation

16 position injector and 150 sample tray– 16 position injector and 150 sample tray– Removable 50 ml vial racks for easy sample loading and storage

• Automation of common sample prep steps with the 7693A– increases productivity and decreases operator variability

• A new "Multimode" GC inlet provides flexibility:– Hot or Cold Split, Splitless or Large Volume injections– Facilitates solvent venting, residue venting and backflush– Easy method development for large volume injections