during gc/ms inlet and column maintenance, shutting down ... · analysis time was reduced by more...

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DEANS SWITCH Increase the resolving power of your GC Complex matrices often have too many overlapping compounds to properly resolve analytes of interest. In these cases, additional selectivity is needed. A Deans Switch is an easy – and affordable – way to further resolve multiple components using two different columns in the same analytical run on the same instrument. Additional selectivity can be achieved with two separate detectors. The Agilent CFT Deans Switch offers several unique benefits, including: Low thermal mass that allows the Deans Switch to closely follow the oven ramp Small dead volumes that eliminate peak broadening UltiMetal Plus Flexible metal ferrules and fittings that keep leaks in check, even after many oven temperature cycles Inert surfaces that prevent peak tailing and analyte loss Backflush capabilities that can reduce run times and prolong column life C10:0 Cut C12:0 Cut C14:0 Cut 6.108 6.301 6.482 6.644 6.692 6.760 6.864 7.007 7.127 7.252 7.315 7.378 7.436 7.583 7.768 7.913 7.976 8.030 8.280 8.624 8.989 9.035 9.180 9.736 9.820 6 6.5 7 7.5 8 8.5 9 9.5 Min. 6.109 6.484 6.645 6.694 6.761 6.864 7.009 7.126 7.253 7.316 7.379 7.437 7.583 7.914 7.980 8.027 8.280 8.625 8.988 9.035 9.310 9.736 9.820 9.310 6.167 6.165 Analysis of FAME content and distribution in biodiesel blends using heart-cutting 2D gas chromatography Top: Biodiesel separation on the primary column before the heart-cuts. Bottom: Separation after the heart-cuts. FLOW SPLITTERS Gather more data in less time Analyzing complex samples may require using different GC detectors to meet detection limits, overcome matrix interferences, or confirm unknown peaks. A CFT splitter – which splits effluent from a single column to two or three detectors on the same GC – is a time-saving alternative. However, this technique can be hampered by technical limitations of the splitting hardware. Agilent CFT Splitters solve these challenges with leading-edge innovations like these: The column and restrictors attach to the module using UltiMetal Plus Flexible metal ferrules that do not outgas, shed, detach, or leak – even after multiple oven cycles All surfaces are deactivated as part of the Inert Flow Path Aux EPC allows for optimal flow to GC and MS detectors on the same system Calculator determines the correct restrictor dimensions for a specific split ratio Heavies past end of acquisition are backflushed 1. Cotinine 2. Meprobamate 3. Carisoprodol 4. Caffeine 5. Theobromine 6. ISTD 7. Doxepin (Trans) 8. Sertraline 9. ? 10. Diazepam 11. Hydrocodone 12. Nordiazepam 13. Fentanyl Scan-TIC NPD SIM-ion 245 (Fentanyl Target Ion) 1 2 3 4 5 6 7 89 10 11 12 13 Screening of a whole blood sample Analysis time was reduced by more than 85%, not including the time saved by using DRS. Two-dimensional GC (GC x GC) is a powerful technique that can separate very complex mixtures – such as those found in hydrocarbon processing, environmental, and food/fragrance applications. The Agilent GC x GC method uses two columns, typically of very different polarities, installed in series with a differential flow modulator between them. Four key properties of the modulator are: Requires no cryo-cooling to re-focus, providing significant savings to the lab Collects the material from the first column, dividing the peak into several cuts Focuses the material collected from each cut into a narrow band Introduces the bands sequentially into the second column GC X GC FLOW MODULATOR 2D data for complex mixtures 3-ring 2 -rin g 1 -rin g 3-ring 2 -rin g n-C22 Monomethyl branched n-C21 Flow modulation applied to a gas oil feedstock The peak-generating ability of GC x GC is much greater than that of a single-column separation. High-boiling sample matrix components must be fully eluted before starting your next run. This usually means adding a bakeout routine to the end of your method – which can dramatically increase cycle times. Using Agilent CFT Backflush configurations eliminates the need for bakeout by reversing column flow, resulting in: • Higher productivity through shorter analytical run times • Less maintenance: Removing high boilers reduces the need for column trimming, detector maintenance, and recalibration • Lower operating costs: Columns last longer when they are not exposed to high-temperature bakeout routines – or the build-up of high-boiling compounds • Better data: Continual system contamination is minimized to ensure long term data quality CFT BACKFLUSH Reduce run time and increase throughput Run ended at 42 minutes, and included a 7 min. backflush period at 280 °C column temperature. It took an additional 33 min and heating the column to 320 °C to remove the late eluting matrix components, which are not the focus of the analysis. showing the column was clean Blank run after backflushing 5 10 10 20 25 30 35 40 45 50 55 60 65 70 min Cycle time shortened by more than 30% Here, backflush reduced both cycle time and sample carryover. Ion source contamination was also minimized, because no heavy residues were introduced into the MSD. AGILENT CAPILLARY FLOW TECHNOLOGY MULTIPLY YOUR GC AND GC/MS CAPABILITIES AND DIMENSIONS Capillary Flow Technology (CFT) solves a problem that chromatographers have wrestled with for decades: creating inert, leak-free capillary connections that withstand the extreme temperatures of a modern GC oven. CFT devices are part of the Inert Flow Path, with low thermal mass and small dead volume. When used with the UltiMetal Plus Flexible metal ferrules, they provide the most secure connections while precisely diverting your gas flows. This opens the door to techniques that can expand analytical capabilities, improve your results, and conserve both time and resources. Visit agilent.com/chem/CapillaryFlowTechnology to learn how to increase productivity and solve difficult application problems This information is subject to change without notice. © Agilent Technologies, Inc., 2014 Printed in the USA, July 22, 2014 5991-4724EN During GC/MS inlet and column maintenance, shutting down the MS for system cooling and venting can cause significant downtime. The Agilent Purged Ultimate Union eliminates the need for cooling and venting by providing simple backflush capabilities to an existing GC or GC/MS method. This enables: Simple leak-free connections, part of the Inert Flow Path Risk-free inlet and column maintenance by preventing air from entering the MSD Simple backflush resulting in shorter analysis times and increased throughput by removing matrix contamination from the system PURGED UNIONS Fast routine maintenance and simple backflush Purged Ultimate Union configuration for rapid and universal GC/MS backflushing, applied to selected reaction monitoring. Control the backflush flow during inlet and column maintenance to avoid venting the MS. 7890B GC 5977A Series GC/MSD

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Page 1: During GC/MS inlet and column maintenance, shutting down ... · Analysis time was reduced by more than 85%, not including the time saved by using DRS. Two-dimensional GC (GC x GC)

DEANS SWITCH Increase the resolving power of your GC

Complex matrices often have too many overlapping compounds to properly resolve analytes of interest. In these cases, additional selectivity is needed.

A Deans Switch is an easy – and affordable – way to further resolve multiple components using two different columns in the same analytical run on the same instrument. Additional selectivity can be achieved with two separate detectors. The Agilent CFT Deans Switch offers several unique benefits, including:• Low thermal mass that allows the Deans Switch to closely

follow the oven ramp• Small dead volumes that eliminate peak broadening• UltiMetal Plus Flexible metal ferrules and fittings that keep

leaks in check, even after many oven temperature cycles• Inert surfaces that prevent peak tailing and analyte loss• Backflush capabilities that can reduce run times and prolong

column life

C10

:0 C

ut

C12

:0 C

ut

C14

:0 C

ut

6.10

8

6.30

1

6.48

2

6.64

46.

692

6.76

0

6.86

4

7.00

7

7.12

7

7.25

27.

315

7.37

87.

436

7.58

3

7.76

8

7.91

37.

976

8.03

0

8.28

0

8.62

4

8.98

9

9.03

5

9.18

0

9.73

6

9.82

0

6 6.5 7 7.5 8 8.5 9 9.5 Min.

6.10

9

6.48

4

6.64

56.

694

6.76

1

6.86

4

7.00

9

7.12

6

7.25

37.

316

7.37

97.

437

7.58

3

7.91

47.

980

8.02

7

8.28

0

8.62

5

8.98

8

9.03

5

9.31

0

9.73

6

9.82

0

9.31

0

6.16

76.

165

Analysis of FAME content and distribution in biodiesel blends using heart-cutting 2D gas chromatography

Top: Biodiesel separation on the primary column before the heart-cuts. Bottom: Separation after the heart-cuts.

FLOW SPLITTERS Gather more data in less time

Analyzing complex samples may require using different GC detectors to meet detection limits, overcome matrix interferences, or confirm unknown peaks.

A CFT splitter – which splits effluent from a single column to two or three detectors on the same GC – is a time-saving alternative. However, this technique can be hampered by technical limitations of the splitting hardware. Agilent CFT Splitters solve these challenges with leading-edge innovations like these: • The column and restrictors attach to the module using

UltiMetal Plus Flexible metal ferrules that do not outgas, shed, detach, or leak – even after multiple oven cycles

• All surfaces are deactivated as part of the Inert Flow Path• Aux EPC allows for optimal flow to GC and MS detectors on

the same system• Calculator determines the correct restrictor dimensions for

a specific split ratio

Heavies past end ofacquisition are backflushed

1. Cotinine2. Meprobamate3. Carisoprodol4. Caffeine5. Theobromine6. ISTD7. Doxepin (Trans)8. Sertraline9. ?10. Diazepam11. Hydrocodone12. Nordiazepam13. Fentanyl

Scan-TIC

NPD

SIM-ion 245 (Fentanyl Target Ion)

1 2

3

4 5

6

7 8 9 101112

13

Screening of a whole blood sample

Analysis time was reduced by more than 85%, not including the time saved by using DRS.

Two-dimensional GC (GC x GC) is a powerful technique that can separate very complex mixtures – such as those found in hydrocarbon processing, environmental, and food/fragrance applications.

The Agilent GC x GC method uses two columns, typically of very different polarities, installed in series with a differential flow modulator between them. Four key properties of the modulator are:

• Requires no cryo-cooling to re-focus, providing significant savings to the lab• Collects the material from the first column, dividing the peak into several cuts• Focuses the material collected from each cut into a narrow band• Introduces the bands sequentially into the second column

GC X GC FLOW MODULATOR 2D data for complex mixtures 3 - r i n g

2 - r i n g

1 - r i n g

3 - r i n g

2 - r i n g

n-C22M o n om e th y l

b ra n c h e d

n-C21

Flow modulation applied to a gas oil feedstock

The peak-generating ability of GC x GC is much greater than that of a single-column separation.

High-boiling sample matrix components must be fully eluted before starting your next run. This usually means adding a bakeout routine to the end of your method – which can dramatically increase cycle times. Using Agilent CFT Backflush configurations eliminates the need for bakeout by reversing column flow, resulting in:• Higher productivity through shorter analytical run times• Less maintenance: Removing high boilers reduces the need for

column trimming, detector maintenance, and recalibration• Lower operating costs: Columns last longer when they are not

exposed to high-temperature bakeout routines – or the build-up of high-boiling compounds

• Better data: Continual system contamination is minimized to ensure long term data quality

CFT BACKFLUSH Reduce run time and increase throughput

Run ended at 42 minutes, and includeda 7 min. backflush period at 280 °C

column temperature.

It took an additional 33 minand heating the column to 320 °C

to remove the late elutingmatrix components, which arenot the focus of the analysis.

showing the column was cleanBlank run after backflushing

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

Cycle time shortened by more than 30%Here, backflush reduced both cycle time and sample carryover. Ion source contamination was also minimized, because no heavy residues were introduced into the MSD.

AGILENTCAPILLARY FLOWTECHNOLOGYMULTIPLY YOUR GC AND GC/MS CAPABILITIES AND DIMENSIONS Capillary Flow Technology (CFT) solves a problem that chromatographers have wrestled with for decades: creating inert, leak-free capillary connections that withstand the extreme temperatures of a modern GC oven.

CFT devices are part of the Inert Flow Path, with low thermal mass and small dead volume. When used with the UltiMetal Plus Flexible metal ferrules, they provide the most secure connections while precisely diverting your gas flows.

This opens the door to techniques that can expand analytical capabilities, improve your results, and conserve both time and resources.

Visit agilent.com/chem/CapillaryFlowTechnology to learn how to increase productivity and solve difficult application problems

This information is subject to change without notice.

© Agilent Technologies, Inc., 2014 Printed in the USA, July 22, 2014

5991-4724EN

During GC/MS inlet and column maintenance, shutting down the MS for system cooling and venting can cause significant downtime. The Agilent Purged Ultimate Union eliminates the need for cooling and venting by providing simple backflush capabilities to an existing GC or GC/MS method. This enables: • Simple leak-free connections, part of the Inert Flow Path• Risk-free inlet and column maintenance by preventing air

from entering the MSD• Simple backflush resulting in shorter analysis times and

increased throughput by removing matrix contamination from the system

PURGED UNIONS Fast routine maintenance and simple backflush

Purged Ultimate Union configuration for rapid and universal GC/MS backflushing, applied to selected reaction monitoring.Control the backflush flow during inlet and column maintenance to avoid venting the MS.

7890B GC 5977A Series GC/MSD