what’s new from agilent technologies?s... · new autosampler versus 7683b 7683b 7693a 2-mls l i l...
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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
SR 2-1
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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)
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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 ( )
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
ll f d
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
j
• 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!!