What’s new from Agilent Technologies?Technologies?

Agilent 7693A Automatic Sampler for 7890 and 6890 GC

New Products from Agilent to Enhance Lab Productivityto Enhance Lab Productivity

Agilent Multimode Inlet  Agilent LTM (Low Thermal Mass)for 7890 GC

g ( )Technology 

Agilent Liquid Sampling Portfolio

7683B ALS 7693A ALS

G2880 ALS CTC Pal 

New 7693A Automatic Liquid Sampling System

L h d M h 2009Launched March 2009

New Tray with 150 Vial Positions

New Injector with 16 Vial Positions Vial PositionsVial Positions

Upgradeable Platform (7693A) Based on Latest Technology: Grounds‐Up RedesignTechnology: Grounds Up RedesignNew syringe carriage design 

• Rack & pinion drive, stronger motor, no belts

Smarter instrument with feedback loops

Improved motors

A new active gripperA new active gripper 

• With additional motor 

All new electronics

• Smaller, more reliable, extended capabilities

Higher capacity

• Physically larger to handle more and larger vials

Improved reliability

• Longer mean‐time before first failure

Compatibility with all 6890 GCsCompatibility with all 6890 GCs

New Autosampler versus 7683B

7683B 7693A

2 L S l i l ALS T O l 8 162-mL Sample vials, ALS Tower Only 8 16

2-mL Sample vials with Tray 100 150

Usable solvent capacity 6 x 4mL 10 x 4mLUsable solvent capacity 6 x 4mL 10 x 4mL

Injection volume settings 6 49

Maximum syringe size 100 µL 500 µLa u sy ge s e 00 µ 500 µ

Dual simultaneous injection Yes Yes

Bar code reader Yes Yes

Sandwich injections No Yes

Sample prep capabilities No Yes

7693A Injector & Tray Features

16 (I j t ) d 150 (T ) 2 L l16 (Injector) and 150 (Tray) , 2‐mL samples

Removable, 50‐vial sample trays

Injections from 1‐50% of syringe size in

Setting (injecting into S/SL inlet)

Precision (%RSD)

Injections from 1‐50% of syringe size in1% increments

Modular, field repairable 

20% to 50% 0.30%10% 0.80%2% 1-2%

• Self Calibrating, alignment like 7683B

• LVI (Large Volume Injection to 250 µL per injection)

1% 3-5% • Single Sample Heater,  Barcode reader/mixer

• Active gripper

• Compatible with all 6890, 7890, 7820 and 6850 (I j t O l f 6850)(Injector Only for 6850)

• Optional heater/chiller plate (requires circulating bath)

16 Sample Capacity in 7693A Injection Tower

7673 7683 76937673 7683 7693

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

New ALS ChemStation Parameter Screen

Sandwich Injections with 7693A

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

Sample Prep Programming Flexibility 

• Sandwich injections (up to 3 layers with air gap)

• Examples of simple liquid manipulation

– ISTD addition

– Reconstitution

Mi i (R i B C d R d / H t / Mi ti )– Mixing (Requires Bar Code Reader / Heater / Mixer option)

– Dilution

– Derivatization

– 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

7693A Software for Sample Handling 

Compare Manual prep vs 7693A prep%RSDs of RRFs from 7 level calibration%RSDs of RRFs from 7 level calibration

7693A is as good as a skilled chemist when making a 7‐level calibration set7 level calibration set

50

60

70

20

30

40Manual 1-1

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Summary of Key Improvements, 7683B to 7693A

100% increased vial capacity on the standard turret

50% higher vial capacity of the tray50% higher vial capacity of the tray

Injection volume increments improved from 10% of syringe volume to 1% of syringe volume for greater precisionvolume to 1% of syringe volume for greater precision

250 µL single stroke injection allowed on 7693A* vs 50 µL on 7683B7683B

New Heating and Mixing Capability

Automated Sample PrepAutomated Sample Prep

* Requires Enhanced Sample Handling Syringe Carriage* Requires Enhanced Sample Handling Syringe Carriage

New Multimode Inlet for Gas Chromatography

Agilent’s New Programmable (Multimode) Inlet

7890 standard

7890 turn‐top for easy liner exchange

7890 standard pneumatics

Uses 7890 S/SL liners, septa, ferrules and o‐rings

Air plus liquid CO2, N2cryogenic cooling

rings

Interchangeable conditions and consumables with current S/SL, while having the ability g / , g yto do advanced techniques when / if needed

Multimode Inlet Solves Many Problems 

Performing large volume injection (LVI) of relatively clean samples?

• Programmable injection matches solvent evaporation rate and maximizes analyte• Programmable injection matches solvent evaporation rate and maximizes  analytetransfer into the column/detector

• Decrease MDL by injecting more sample 

Injecting dirty samples?

• Matrix vent, backflush and easy liner changing minimize dirty sample affects

/Performing analyses of high molecular weight and/or thermally labile compounds?

• Temperature programming of Multimode inlet elutes analytes at the lowest• Temperature programming of Multimode inlet elutes analytes at the lowest possible temperature, minimizing breakdown and absorption

• Discrimination of high molecular weight compounds is minimal  

New Multimode Inlet Features HardwareHardware

Temperature range of ‐160 oC to 450 oC

Heating @ 15 oC/sec

S t /Li E il E h bl i T T I l tSeptum/Liner Easily Exchangeable using Turn‐Top Inlet

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

Support for single stroke injections from 0 1 μL to 250 μLSupport for single stroke injections from 0.1 μL to 250 μL

EPC Compatible with Packed Liners

Compatible with 7890A, 7683, CTC Combi PAL

Software

Ten temperature ramps

Wizard for setting up large volume injections

Fully integrated into ChemStation, MSD ChemStation, EZChrom, and MassHunter

Multimode Inlet ‐ Cold Injections

No syringe‐needle discrimination

• Minimal inlet discrimination 

No special syringes, liners or consumables No special syringes, liners or consumables 

Large volume injection (5 µL to 250 µL)

• Lower detection limits

Solvent vent/matrix vent 

• Decrease interference / maintenance 

FlexibilityFlexibility

• Hot/cold split/splitless, temperature programmed vaporization

Cold trapping in liner

• Improves chromatographic peak shape, resolution

Capillary column backflush with Capillary Flow Technology 

• Decreases cycle time, maintenanceDecreases cycle time, maintenance

Multimode Inlet ‐ Solvent Vent Mode for Large Volume InjectionInjection

Set inlet temperature at or below solvent boiling point

Syringeneedle

• But, what Temperature

Set high split ratio

• But, what split ratio?

Liner

Carrier

, p

Inject sample very slowly into PTV

• How slowly

Solvent evaporates through split vent

Vent

Solvent evaporates through split vent

• At what rate?

Close split vent and ramp PTV temperatureSampleAnalyteSolvent

• When?

Carry out separation on analytical columnColumn

PTV Cold Splitless and SV – Temperatureand Flow Programsand Flow Programs

Transfer of sample from inlet to column GC Separation

Cold Injection

PTV Temp 20 350

PTV cooldown

0.9 minLarge volume injections used to i l t f th d d l tPTV Temp

GC Oven Oven = 40Oven ramps

20 350require a lot of method development 

GC OvenTemp

P

purge flow = 30

Oven = 40

Inlet = 11.40 psiNot Now!

PurgeStatus purge off purge on

0 0.05 2.5 26Min 1.50.6

Built‐in Wizard for Solvent Vent Method Development

Solvent Elimination Calculation WizardStep 1‐ Enter Solvent of Choice and Injection VolumeStep 1 Enter Solvent of Choice and Injection Volume

Step 2 ‐Wizard Calculates the Injection Rate and Vent Time According to the Selected Inlet Temperature and Vent Flow

Step 3 ‐ Confirm Values Suggested by the Wizard and Save Parameters to ChemStation MethodParameters  to ChemStation Method

All inlet &injection parameters determined for youdetermined for you 

Cold Splitless Injection Really Works – Inject up to 10 µL (liner dependent) without Solvent Vent(liner dependent) without Solvent Vent

280 oCHoldInject

700 C/ i

Injectup to 10 µL

60 oC or lower

700 oC/min

60 C or lower0.1 min

Multimode Injection LVI of Triazine Herbicides 

1 µL Cold Splitless injection

1 µL 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 1.33263 1.33

compoundgives largest

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

Improved Sensitivity for Semi‐volatiles in Drinking Water

Cold Splitless Areas for 1 2 3 4 5 µL InjectionsCold Splitless Areas for 1, 2, 3, 4, 5 µL Injections normalized to 1 µL Hot Splitless Injection

Areaincrease

Normali ed hot splitless area 1

using cold splitless

Normalized hot splitless area = 1

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

Mire

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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 ( )

High Temperature Simulated Distillation using Agilent's New Multimode InletAgilent s New Multimode Inlet

C20 marker

C92

5 10 15 20 25 30

Agilent LTM (Low Thermal Mass)Rapid Heating/Cooling System for GC, GC/MSRapid Heating/Cooling System for GC, GC/MS

Typical Cooling Times for a 5” LTM Column

oC 2 m 5 m 10 m 15 m 30 m

Column Length

350->300 3 5 6 7 9300->250 3 5 7 7 13250->200 4 7 8 10 17200->150 4 8 11 13 22150->100 7 13 17 19 36100->50 13 27 34 41 75

Type Time350oC  50C LTM (2m Column)   34 seconds         (= 3+3+4+4+7+13)Equilibration 3 secondsEquilibration 3 seconds

350oC  50C 7890 GC 3‐4 minutesEquilibration 2‐3 minutes

Interfacing LTM to an Agilent GC

Modules outside isothermal GC oven for fast heating/cooling

Use same GC injectors, detectors, autosamplers, software, …

Independent and simultaneous temperature programming of: 1 2 col modules (standard size fastest)1‐2 col modules (standard size, fastest) 1‐4 col modules (small size)

LTM Column ModulesLTM Column Modules(standard width shown))LTM Control System w/ Keypad User Interface… Agilent Control SW Now Available… Agilent Control SW Now Available

Fast Simulated Distillation Under 3 Minutes ‐ Productivity 

pA

2000 ASTM D2887 Reference Oil

1000

1500 RVM oven : 45ºC to 350ºC at 150ºC/min

pA 12

min0.25 0.5 0.75 1 1.25 1.5 1.75 20

500

pA

4000

5000

6000

C5 C

10

C

C14

C16

6 f t d t

Calibration sample C5‐C44

RVM oven : 45ºC to 350ºC at 150ºC/min

1000

2000

3000

C6 C

7C

8 C 9 C11

C15

C17

C18

C20

C24

C28 C

32

C36

C40

… 6x faster compared to conventional ASTM D2887 procedure

0min0.25 0.5 0.75 1 1.25 1.5 1.75 2 2.25

Fast Simulated Distillation Under 3 Minutes ‐ Repeatibility

pA

9 0 0

6 0 0

7 0 0

8 0 0

Creaked gas oil, diluted 1:3  in pentaneRVM oven : 45ºC to 350ºC at 

3 0 0

4 0 0

5 0 0150ºC/min

0

1 0 0

2 0 0

m in0 0 .5 1 1 .5 2 2 .50

Chromatographic overlay of 10 runs shows outstanding repeatability

Retention Time RepeatabilityC14 to C17 Hydrocarbons

35 C to 350 C @ 50 C/min.RT Height Area PK WidthRT Height Area PK Width

C14 Average 3.173296 28692.6 24991.85 0.017406C14 SD 0.000956 276.1011 559.829 0.000284C14 RSD 0.030124 0.962273 2.240046 1.633047C15 Average 3.448155 11586.31 11512.6 0.016083C15 SD 0.001137 119.7229 154.8721 0.000554C15 RSD 0.032977 1.033314 1.34524 3.444738C16 Average 3.721938 23307.99 20345.54 0.017783gC16 SD 0.001384 224.5316 389.5163 0.00069C16 RSD 0.037178 0.963325 1.914504 3.879877C17 Average 3.974779 23356.03 19971.48 0.017978C17 SD 0 001351 239 7177 299 2454 0 000562C17 SD 0.001351 239.7177 299.2454 0.000562C17 RSD 0.033989 1.026363 1.498364 3.127652

Based on 10 runs

Retention Time RepeatabilityC14 to C17 Hydrocarbons

35 C to 350 C @ 100 C/min.RT Height Area PK Width

C14 A 1 888362 12160 46 19415 62 0 010308C14 Average 1.888362 12160.46 19415.62 0.010308C14 SD 0.000261 124.2667 312.7175 8.91E-05C14 RSD 0.013798 1.021891 1.610649 0.863997C15 Average 2.031785 4918.886 8113.916 0.010073C15 SD 0.000189 49.98891 87.93099 4.06E-05C15 RSD 0.009323 1.016265 1.083706 0.402904C16 Average 2.170917 9772.619 15728.54 0.010249C16 SD 0.000259 101.5109 127.1452 3.25E-05C16 RSD 0.011925 1.038727 0.808372 0.316714C17 Average 2.300579 9841.635 15477.91 0.010418C17 SD 0.000409 198.2333 178.3228 0.000118C17 RSD 0.017777 2.014231 1.152111 1.136056

Based on 10 runs

Retention Time RepeatabilityC5 to C40 Mix

45 C to 350 C @ 250 C/minHydrocarbon C5 C6 C7 C8 C9 C10 C11 C12 C14 C15RT 0.13676 0.17327 0.22944 0.30102 0.3786 0.45672 0.53111 0.60298 0.73073 0.78855SD 0.00018 0.00018 0.00015 0.00013 0.00013 0.00026 0.0002 0.00027 0.00028 0.00031%RSD 0.13178 0.10606 0.06457 0.04204 0.03505 0.05801 0.03798 0.04518 0.03889 0.03894

Hydrocarbon C16 C17 C18 C20 C24 C28 C32 C36 C40RT 0.84418 0.89529 0.9439 1.03433 1.19225 1.34146 1.5513 1.90969 2.57287SD 0 00036 0 0003 0 00037 0 0003 0 00046 0 00079 0 00132 0 00181 0 00377

Based on 10 runs

SD 0.00036 0.0003 0.00037 0.0003 0.00046 0.00079 0.00132 0.00181 0.00377%RSD 0.04321 0.03306 0.03939 0.02915 0.03828 0.05917 0.08512 0.09457 0.14667

Retention Time Repeatability

Retention time repeatability as tested with a C14 to C17 probe ranges from 0.01 to approximately 0.03% RSD

Retention time repeatability is in the above range

• Even with starting column temperatures of 35o C

RT repeatability actually improves at higher oven ramp ratesRT repeatability actually improves at higher oven ramp rates

Wide boiling range hydrocarbons (C5 to C40) also shows very good RT stability

/• RSD of approximately 0.03 to 0.10 using a rapid temperature program of 250o C/min ramped from 45o C to 350oC

Overall, for most analytes, expected RT repeatability is similar to that obtained from conventional air‐bath ovensobtained from conventional air bath ovens

These results illustrate the lack of cold spots and highlight good uniformity in the LTM column module

Using LTM and backflush to improve productivity

The measurement of polycyclic (polynuclear) aromatic hydrocarbons (PAHs) by GC‐MS is one of the most important applications in environmental analysis.

In most reference methods, for instance the  U.S. EPA Methods 525, 625 and 8270 target 16 separate PAHs625, and 8270 target 16 separate PAHs. 

• Other semivolatile compounds can complicate quantification so analysis time can be relatively long (20 to 30 mins). 

• Simply using a GC column with a smaller diameter speeds things up, but care has to be exercised if the separation of regulated PAH isomers is not to be compromised

Th LTM d b kfl h i A il t’ C ill Fl t h lThe LTM and backflush using Agilent’s Capillary Flow technology can make significant improvements in sample throughput

System configuration for PAH measurements

Inlet EPC Aux

EPCQ i kSGC OvenP1

Retention Gap

EPC

P2

QuickSwap

Retention Gap

GC Oven

S/S Inletp

50 cm X 250 μmp

50 cm X 250 μm

Restrictor17 cm X 110 μm

MSDSystem configuration for fast GC analysis of PAHs using an 

18 m X 180 μm X 0.18 μm DB5-MS

LTM M d l

MSDy gLTMmodule and QuickSwap device for backflush.

LTM Module

PAH Reference Method Reference method: 30 m x 0.25 mm ID x 0.25 µm HP‐5MSGC‐MS in scan/SIM – scan trace

Abundance

Elution Mean tROrder Compound name (min) sigma % RSD 1 Naphthalene 2.850 0.000 0.00 2 Acenaphthylene 3.280 0.000 0.00 3 Acenaphthene 3.326 0.000 0.00 4 Fluorene 3.481 0.000 0.00 5 Phenanthrene 3 825 0 000 0 01

2

3

43000000

3500000

4000000 5 Phenanthrene 3.825 0.000 0.01 6 Anthracene 3.846 0.000 0.00 7 Fluoranthene 4.429 0.001 0.01 8 Pyrene 4.583 0.001 0.01 9 Benz(a)anthracene 5.654 0.001 0.02 10 Chrysene 5.693 0.001 0.0111 Benzo(b)fluoranthene 6.979 0.001 0.02

875-61

2000000

2500000

3000000 ( )12 Benzo(k)fluoranthene 7.016 0.002 0.02 13 Benzo(a)pyrene 7.405 0.002 0.02 14 Indeno(123-cd)pyrene 8.910 0.002 0.02 15 Dibenz(ah)anthracene 8.968 0.002 0.02 16 Benzo(ghi)perylene 9.278 0.002 0.02

Average 0 001 0 01

161513

11-129-101000000

1500000

2000000 Average 0.001 0.01

1614

3

4 00 6 00 8 00 10 00 12 00 14 00 16 00 18 00 20 000

500000

Time--> 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00Time-->

Translated FAST PAH methodLTM method: 20 m x 0.18 mm ID x 0.18 µm DB‐5MSGC‐MS in scan/SIM – SIM trace – BF at 10 min

Abundance

9500000

Table 4. Area Repeatability for Target PAHs Order Mean of elution Compound name peak area % RSD

1 Naphthalene 2145022 45438.72 2.122 Acenaphthylene 2531734 57007.60 2.25 3 A hth 3410703 76081 85 2 23

3

45 6

7500000

85000003 Acenaphthene 3410703 76081.85 2.23 4 Fluorene 3108369 66651.55 2.14 5 Phenanthrene 2341505 50290.78 2.15 6 Anthracene 2304885 46774.62 2.03 7 Fluoranthene 2598819 57961.99 2.23 8 Pyrene 2678698 58471.60 2.18 9 Benz(a)anthracene 2264966 58416.06 2.58 10 Chrysene 2597444 50507 12 1 94

2

87

5-61

4500000

5500000

6500000 10 Chrysene 2597444 50507.12 1.94 11 Benzo(b)fluoranthene 2245073 50491.19 2.25 12 Benzo(k)fluoranthene 2954729 71902.33 2.43 13 Benzo(a)pyrene 2239967 57434.91 2.56 14 Indeno(123-cd)pyrene 1616395 56133.34 3.47 15 Dibenz(ah)anthracene 3065828 86273.62 2.81 16 Benzo(ghi)perylene 2511598 65387.08 2.60

116

2

15

1311-129-10

2500000

3500000Average 2.37

14

5

Time >

500000

1500000

2 00 3 00 4 00 5 00 6 00 7 00 8 00 9 00Time--> 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00

FAST LTM method with backflush – Soil extract

FLTM method 20 m 0 18 mm ID 0 18 m DB 5MS

1 6e+07

Abundance800000

FLTM method: 20 m x 0.18 mm ID x 0.18 µm DB‐5MSGC‐MS in scan/SIM – SIM trace Sample (soil extract) – BF at 10 min.

7

5-6

1.2e+07

1.4e+07

1.6e+07

9-10600000

700000

48

7

8000000

1e+07

1511-12

Benzo(e)pyrene300000

400000

500000

4000000

6000000

16

151413

100000

200000

9-1012000000

Time--> 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00

5.50 6.00 6.50 7.00 7.50 8.00 8.50 9.00 9.50

Blank after run – without backflush

1450000Abundance

LTM method: 20 m x 0.18 mm ID x 0.18 µm DB‐5MSGC‐MS in scan/SIM – scan trace Blank after run without back‐flush

1050000

1250000

650000

850000

250000

450000

2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00

50000

250000

Time-->

Comparing blanks with and without backflush

1450000Abundance

LTM method: 20 m x 0.18 mm ID x 0.18 µm DB‐5MSGC‐MS in scan/SIM – scan trace Blank after run without back‐flush

1050000

1250000

Without backflush

650000

850000backflush

250000

450000

With backflush

2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00

50000

250000

Time-->

Agilent's New Gas Phase ProductsAgilent’s New 7820 GC A New "Multimode" GC inlet providesAgilent s New 7820 GC

• Competitively priced mid range GC

• Superb  performance

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A New Multimode  GC inlet provides flexibility:

• Hot or Cold Split, Splitless or Large Volume injections

• Fully featured

– EPC, ALS, choice of detectors etc.

• Simplified user interface for improved ease of use

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• Facilitates solvent venting, residue venting and backflush

• Easy method development for large volume i j tiuse

Agilent's New 7693A ALS 

• Increases sample throughput

l ll

injections

New Low Thermal Mass System

• Rapid heating/cooling– Auto‐alignment, easy installation

– 16 position injector and 150 sample tray

– Removable 50‐vial racks for easy sample loading and storage

• Available for GC and GC/MS

• No compromise in flexibility

– Use same GC injectors, detectors, ALS etc.loading and storage

• Automates common sample prep steps with the 7693A

– Increases productivity and decreases operator variability

Summary

Over the past 5 years, Agilent has demonstrated true innovation with the launch of new instruments, accessories and column technologies, g

In 2009, the introduction of a new competitively priced GC, new ALS, flexible multimode injector, fast GC,  1290 LC and 7100 CE illustrates that this innovation continues in separation sciences

Agilent’s track record in advanced MS technologies is well d d d i i h h l h h d f 2008 f hdocumented and continues with the launch at the end of 2008 of the GC/MS/MS

Keep tuned for other exciting product launches!!Keep tuned for other exciting product launches!!