Topic 8 Low Thermal Mass and Capillary Flow Technology … · Low Thermal Mass and Capillary Flow Technology for Faster Cycle Times ... – Less frequent and faster GC & MSD maintenance

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Welcome toNEW “Chromatography Tips & Trick” India Seminar tour

Low Thermal Mass and Capillary Flow Technology for Faster Cycle Times

Abhijit PalMarketing Program Manager , India Chemical Analysis Solution

Life Sciences and Chemical Analysis Agilent Technologies , India

Goa 4 th May , 2010

Group/Presentation TitleAgilent Restricted

Month ##, 200X

AgendaSignificantly Reduce Analysis Times:

• Avoiding Bake-Out of HeavyComponents Beyond Your Peaks of Interest

• Rapid Heating and Cooling

GC, GC/MS News

… Using Agilent’s Technologies:

“Backflush” via Capillary Flow Devices

Low Thermal Mass (LTM) System

Both sold with new 7890 GC, GC/MS…but existing 7890/6890 systems canalso be upgraded to utilize these “productivity” technologies

Agilent’s Newest Technologies:

• Blos bead for GC/NPD

• Triple-axis detector for GC/MSD

• Agilent 7010 GC/MS/MS

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Defining Productivity

• More analyses per unit time . . .

– Faster and more efficient separations– Shorter analysis cycle time (time from injection to injection) – Reduced requirement for sample preparation

• with consistently better results . . .

– Quantitative: accuracy, precision, detection limits, linear range– Qualitative: response ratios, confirmatory retention times, library

searches (eliminate false negatives and false positives)

• while using less operator time for each analysis.

– Less time performing maintenance– Extensive computer control and data processing– Simplified operator review/approval

Productivity: the Sum of Many Technologies

• Low Thermal Mass GC

• Capillary Flow Technology - Backflush

• Hydrogen carrier gas for GC and GC/MS

• Retention Time Locking (RTL) Editor (& Methods)

– With more RTL Databases

• Trace Ion Detection

• Fast Electronic - Synchronous SIM/Scan

• Method Translator

• High signal-to-noise Triple-Axis Detector

– Gain Normalization of the EM

– EM Saver

• 2nd Generation Deconvolution Reporting Software (DRS)

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Jan 2007

Capillary Flow Technology

• Proprietary technology for GC IN OVEN flow manipulation

• Benefits

• Examples

– Backflush

– QuickSwap

– Deans Switch (Heart-cutting)

– Splitters

•

Capillary FlowTechnology Suite

Jan 2007

Significance of Capillary Flow Technology

• Customer survey

#1 in customer ranking• Customer comment

“Change the way we do chromatography, this is a lock-out for Agilent…Emphasize how simple it is:

- Agilent = Plate,- Shimadzu/Thermo = 30 parts”

• Agilent GC Field Advisory Team

Agilent 7890A’s key contribution

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Jan 2007

Improvements with Agilent 7890A GC

• Proven in Agilent 6890 GC

• Improvements in Agilent 7890 GC

– New capabilities

– Easier to set-up and operate

– Backflush user interface in software

• Improvements in support

– Application notes

– AE training

– CE training

GOAL: Widespread lockout for Agilent GC and GC/MS

Jan 2007

Capillary Flow Technology – Many Capabilities

QuickSwap (GC/MS)- Inlet maintenance, change GC column, without venting MS** Shorten/eliminate GC/MS downtime

Solvent Bypass - Eliminate early peaks** Lower detector maintenance costs

Heart Cut- Cut peaks to another column** Find trace levels in a complex matrix

Backflush- Eliminate later/post-run peaks** Shorten cycle times, eliminate sample carryover, less

column usage & lower detector maintenance costs

Split- Send all peaks to multiple detectors** Obtain more information during each run.

Find peaks of interest in unknowns

Modulate (New)- Send faction of effluence to 2nd column few seconds a time** Extra dimension separation during each run

obtain much rich information for complex sample

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Month ##, 200X

Obtaining Faster GC, GC/MS Analytical Cycle Times – A Variety of Approaches to Fit Your Lab and Your N eeds

Post-RunBake-Out

ChromatographicRun

Post-RunCool-Down

Pre-RunALS Set-Up


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Post-RunBake-Out

ChromatographicRun

Post-RunCool-Down

Pre-RunALS Set-Up

Included “ALS Sample Overlap” 7890 GCin in ChemStation SW Faster Cool-down

HW/SW

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Month ##, 200X


Post-RunBake-Out

ChromatographicRun

Post-RunCool-Down

Pre-RunALS Set-Up


HW/SW

Faster GC Column Selection,Analyses Method Translation


Month ##, 200X


Post-RunBake-Out

ChromatographicRun

Post-RunCool-Down

Pre-RunALS Set-Up


HW/SW

Faster GC Column Selection,Analyses Method Translation

GC Add-Ons Capillary Flow TechnologySignficantly Faster GC (Backflush)Analytical Cycle Times

LTM Technology LTM Technology(Rapid Heating) (Rapid Cooling )

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5 10 15 20 25 30 35 40 45 50 55 60 65 70

It took additional 33 minsand column to 320oC to remove these high boilers.

min

Milk Extract


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Backflush During GC Run

S/S Inlet

Purged CFTDeviceColumn

25 psi

4 psi

MSD

Aux EPCSplit Vent Trap

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Backflush

S/S Inlet


1 psi

45 psi

MSD


During GC Run

After GC Run

S/S Inlet


25 psi

4 psi

MSD



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5 10 15 20 25 30 35 40 45 50 55 60 65 70

Run stopped at 42 min and backflushed at 280oC for 7 mins.

It took additional 33 minsand column to 320oC to remove these high boilers.

Blank run after backflushing

min

showing the column was clean.

Milk Extract

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Benefits of Backflushing

– More samples/day/instrument

– Better quality data

– Lower operating costs

– Less frequent and faster GC & MSD maintenance

– Longer column life

– Less chemical background

– Available for Agilent 6890/7890


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GC and GC/MS Productivity Gains with Backflush

Industry Application Cap Flow Device

Back-flush Time

Saved

Cool-Down Time

Saved

FoodSafety

Pesticides inMilk Extract

Splitter 26 min(30%)

1 min

Enviro Fast 8270 QuickSwap 20 min (50%)

3 min

Forensics Fast Drugs of Abuse

Splitter 13 min

(20%)

1 min

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Each Purged Capillary Flow Device Has Dual Use

Backflushing

– Removes heavies from column

- Plus -

QuickSwap - Remove column w/o venting

– Air & H 2O blocked

– Safe disconnection of column from inlet for inlet maintenance

– Reversed flow through column during inlet maintenance

– Maintain constant flow to MSD

(flow rates exceeding 2 mL/min require an MSD with Performance Turbo)

MSD TransferLine

Aux EPC In

Column Effluent


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Other Purged Capillary Flow Devices AlsoProvide Dual Use (including Backflush Capability)

22--Way Splitter with Way Splitter with MakeupMakeup

33--Way Splitter with Way Splitter with MakeupMakeup

Deans SwitchDeans Switch

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Pesticides: Three Way Splitter with Makeup

1X method with 1:1:0.1 split FPD:MSD:ECD

3-Way Splitter with Makeup

Auto-sampler

7890GC

Column

Phosphorus FPD

30 m X 0.25 mm id X 0.25 um HP-5MS

5975C MSD

uECDAUX EPC3.8 psig


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Full scan TIC

SIM

µECD

5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00

FPD(P)

Milk Extract (1 injection)

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“LTM” (L ow Thermal M ass) Technology (Patented)

Directly heat/cool fused silica GC columns

“LTM” (L ow Thermal M ass) Technology

•Direct heating of fused silica GC columns

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Interfacing LTM GC to an Agilent 7890 or 6890 GC

GC oven door replaced with LTM-ready GC oven door (easy) Use same GC injectors, detectors, autosamplers, software, …

Column Modules mount outside isothermal GC oven for fast heating and cooling

Independent and simultaneous temperature programming of 1-4 column modules

Note: Front thermal shield removed to show LTM column modulesEntire thermal shield should always be in place during operation

LTM Column Modules

LTM Control System w/ Keypad User Interface(LTM Control SW for ChemStationAvailable from Agilent Nov/Dec’08)


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LTM Heating Speeds

Heating speeds can be set up to1800oC/min

- achievable rates depend on columnmass, configuration and column void times

- … also includeing practical trade-offsof speed vs resolution

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Typical Cooling Times for a LTM Column (Standard Si ze)

oC 2 m 5 m 10 m 15 m 30 m350->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

Column Length

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

350oC � 50C 7890 GC 3-4 minutesEquilibration 2-3 minutes


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Some Practical Uses of LTM Rapid Heating/Cooling

EnvironmentalNeed for high through-put, especially for low margin samples (eg. Total Petroleum Hydrocarbon (TPH)), where analytical cycle times are a critical element in making a profit

Hydrocarbon ProcessingCertain process control analyses (eg. Simulated Distillation) lend themselves to batch analysis. Shorter analytical cycle times get data back to operations faster, or allow more samples/shift

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Month ##, 200XAgilent Restricted

Developing Faster GC Run Times for TPH Analysis(C10�C44 Standard Shown)

2x Faster,7890

min5 10 15 20 25 30 35

pApApApA

020

40

60

80

100n-

C10

n-C

12

n-C

14

n-C

16

n-C

18

n-C

20

n-C

22n-

C23

n-C

24

n-C

26

n-C

28

n-C

30

n-C

32

n-C

36

n-C

40

n-C

44

min2 4 6 8 10 12 14 16 18 20

pApApApA

20

40

60

80

100

120

n-C

10

n-C

12

n-C

14

n-C

16

n-C

18

n-C

20

n-C

22n-

C23

n-C

24

n-C

26

n-C

28

n-C

30

n-C

32

n-C

36

n-C

40

n-C

44

min0.5 1 1.5 2 2.5 3

pApApApA

0

200

400

600

800

1000

n-C

10

n-C

12

n-C

14n-

C16

n-C

18

n-C

20n-

C22

n-C

23n-

C24

n-C

26n-

C28

n-C

30n-

C32

n-C

36

n-C

40 n-C

44

10oC/min30m Column - 7890

20oC/min15m Column - 7890

200oC/min5m Column –LTM/7890 10x Faster,

LTM/7890

StandardGC RunTime


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LTM Also Greatly Reduces Cool-Down Times,� 9x Faster Heating/Cooling Cycle Times

Agilent Restricted

40 min + 5.4 min

20 min + 5.4 min

3 min + 2 min

GC Run Time Cool Down

9x Faster Cycle Time LTM/7890

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Soil Sample by TPH Analysis using LTM/7890Reliable Calculated Results, <3 minute run time

Agilent Restricted

Concentration*

Original Method (30 m) 1097 µg/mL

2X Method (15 m) 920 µg/mL

LTM Method (5 m) 909 µg/mL

*Calculated by Area Sum and Peak Grouping


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pA

0

1000

2000

3000

4000

5000

6000

min0.25 0.5 0.75 1 1.25 1.5 1.75 2 2.25

C5

C6 C

7

C8 C 9

C10

C11

C12

C14

C15

C16

C17

C18

C20

C24

C28 C

32

C36

C40

pA

min0.25 0.5 0.75 1 1.25 1.5 1.75 20

500

1000

1500

2000

Fast Simulated Distillation Under 3 Minutes by Use of Low Thermal Mass (LTM) Technologies… 6x faster compared to conventional ASTM D2887 proc edure

ASTM D2887 Reference Oil

LTM Module : 45ºC to 350ºC at 150ºC/min

Calibration sample C5-C44

LTM Module : 45ºC to 350ºC at 150ºC/min

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LTM System Technology - Summary

• High efficiency temperature programmingfast heatingfast cooling (< 1 min in some configurations)high throughputfast method development

• High performance chromatographyutilize commercially available columns (up to 30m length)very good retention time repeatability

• Easily integrates with conventional Agilent GC utilize existing injectors, detectors

• Multicolumn temperature control (1-4 modules)simultaneous, independent operation multidimensional GChigh throughput parallel systemsstrong synergy with Agilent’s Capillary Flow Technology

• Available for Agilent 6890/7890

ISCC User Meeting

May, 2008Page 34

GC, GC/MS News - Agilent GC/MS Portfolio

Smallest footprint, single GC column

Power of MRM

Industry leading GC/MS System

5975C with 7890GC

7000A GC/MS/MS

5975VL with 6850GC

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High Performance Triple-Axis Detector

Ultra low neutrals noise

Long life and high linearity

“Gain Normalization” corrects tune file for detector aging to allow repeatable, long term method sensitivity

hyperbolic quartztransmission

quadrupoleanalyzer

triple channelelectron multiplier

high energy dynode

steering rod

ion beam

X

Y

OffsetZ

shield for secondary particles

triple channelelectron multiplier

high energy dynode

steering rod

ion beam

XX

YY

OffsetZ

OffsetZ

shield for secondary particles


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Agilent 7000 GC/MS/MS

The best 5975C GC/MS technology: • Heated monolithic gold plated quartz quadrupole

• Proven reliable high performance ion source design

• Low Noise Triple-Axis Detector

The best 6400 LC/MS/MS technology:• Linear acceleration enhanced hexapole collision cell

• MassHunter software

And new helium seeded collision cell technologyFor outstanding performance:

• 100 fg of OFN on column at 100:1 S/N RMS in MS/MS mode

• 500 MRM/sec Speed

Inert, high temp source (same as 5975C)

Triple-Axis Detector(as same 5975)

Gold plated quartz, hyperbolic quadrupole(same as 5975C)

Split Flow Turbo

New high performance hexapole collision cell (proprietary design)

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Topic 8 Low Thermal Mass and Capillary Flow Technology … · Low Thermal Mass and Capillary Flow Technology for Faster Cycle Times ... – Less frequent and faster GC & MSD maintenance