Agilent GC Solutions. A Convenient Deans Switch Method for the Analysis of Permanent Gases in Various Matrices by Gas Chromatography CAG

Transcription

1 Agilent GC Solutions A Convenient Deans Switch Method for the Analysis of Permanent Gases in Various Matrices by Gas Chromatography CAG Shannon Coleman GC Applications October 7, 0

2 Advantages to Using Micro-fluidics for Analysis of Permanent Gases in Various Matrices Simplified design Easier setup Easier maintenance Capillary columns Faster chromatography

3 Example: Bio-Ethanol Fermentation Monitoring

4 System Design: Picking Columns 4

5 J. Sep. Sci. 008,,

6 But wait 6

7 Deans Switch Heart-cutting -D GC provides extremely high chromatograpic resolution Autosampler Cut FID FID Deans Switch Column Column 7890A GC 7

8 Deans Switch. Back Molesieve HP PLOT Q R CAP () PCM P S Restrictor Ch PCM X Ch 8

9 Deans Switch. Back Molesieve HP PLOT Q R CAP () PCM Ch PCM X Ch P S Restrictor 9

10 Deans Switch. Back Molesieve HP PLOT Q R CAP () PCM Ch PCM X Ch P S Restrictor 0

11 System Design System designed for analysis of permanent gases and organics Gas sample valve for sample introduction Split inlet for injection volume control and alternative injection source Deans switch allows for heart cutting permanent gases to Molsieve column Dual detectors for simultaneous analysis from two columns FLOW SOURCE Inl EPC PCM CH = #87X Options OVEN LEFT SIDE 5/86/ 6/86/ INJECTION PORT CAP () Valve System Column Date : Order No : VALVE COMPARTMENT BLOCK BLOCK 4/XXX Col : 9009P-QO, HP-PLOT Q, 5m x 0.mm x 0um Col : 909P-MS4, HP-PLOT Molsieve, 0m x 0.mm x um Restrictor: , Deactivated Fused Silica Tubing, 0.7m x 0. mm /XXX R P S SP options 888 LOOP /XXX 5 6 IN SAMPLE OUT 4 /XXX Column S/N : Item : Restrictor 0.7m x 0.mm Blank FSD Restrictor Tubing Remarks DETECTOR, x0, 05, 06, 09, 70, 75, 860, 888 Bio-ethanol fermentation analysis. Back.

12 Valve Configuration

13 Column Configuration

14 Column Flow 4

15 Column Flow 5

16 Column Flow 6

17 Setting the Heart Cut Time Start with Deans Switch Valve off 7

18 System Operation: Sample Load FLOW INJECTION OVEN LEFT SIDE SOURCE PORT = #87X 5/86/ Valve System Date : Order No : VALVE COMPARTMENT BLOCK BLOCK 4/XXX /XXX S/N : Item : DETECTOR. 5 4 LOOP 6 IN SAMPLE OUT Back Column Inl EPC PCM CH CAP () Column Col : 9009P-QO, HP-PLOT Q, 5m x 0.mm x 0um Col : 909P-MS4, HP-PLOT Molsieve, 0m x 0.mm x um Restrictor: , Deactivated Fused Silica Tubing, 0.7m x 0. mm R P S 888 Restrictor 0.7m x 0.mm Blank FSD Restrictor Tubing 6/86/ /XXX /XXX Options SP options Remarks, x0, 05, 06, 09, 70, 75, 860, 888 Bio-ethanol fermentation analysis. 8

19 System Operation: Sample Inject FLOW INJECTION OVEN LEFT SIDE SOURCE PORT = #87X 5/86/ Valve System Date : Order No : VALVE COMPARTMENT BLOCK BLOCK 4/XXX /XXX S/N : Item : DETECTOR. 5 4 LOOP 6 IN SAMPLE OUT Back Inl EPC PCM CH CAP () H, O, N, CH4, CO, CO, HC s Column Col : 9009P-QO, HP-PLOT Q, 5m x 0.mm x 0um Col : 909P-MS4, HP-PLOT Molsieve, 0m x 0.mm x um Restrictor: , Deactivated Fused Silica Tubing, 0.7m x 0. mm R P S 888 Column Restrictor 0.7m x 0.mm Blank FSD Restrictor Tubing 6/86/ /XXX /XXX Options SP options Remarks, x0, 05, 06, 09, 70, 75, 860, 888 Bio-ethanol fermentation analysis. 9

20 System Operation: FLOW INJECTION OVEN LEFT SIDE SOURCE PORT = #87X 5/86/ Valve System Date : Order No : VALVE COMPARTMENT BLOCK BLOCK 4/XXX /XXX S/N : Item : DETECTOR. 5 4 LOOP 6 IN SAMPLE OUT Back Inl EPC PCM CH Options 6/86/ CAP () Column Col : 9009P-QO, HP-PLOT Q, 5m x 0.mm x 0um Col : 909P-MS4, HP-PLOT Molsieve, 0m x 0.mm x um Restrictor: , Deactivated Fused Silica Tubing, 0.7m x 0. mm /XXX R P S SP options 888 Valve OFF /XXX Column H, O, N, CH4, CO, CO, HC s Restrictor 0.7m x 0.mm Blank FSD Restrictor Tubing Remarks, x0, 05, 06, 09, 70, 75, 860, 888 Bio-ethanol fermentation analysis. 0

21 Finding the Cut Time for the Deans Switch Valve Air 0.8 min Valve ON. min Valve OFF

22 Add Valves Times to Run Time Events Table

23 System Operation: Sample Load FLOW INJECTION OVEN LEFT SIDE SOURCE PORT = #87X 5/86/ Valve System Date : Order No : VALVE COMPARTMENT BLOCK BLOCK 4/XXX /XXX S/N : Item : DETECTOR. 5 4 LOOP 6 IN SAMPLE OUT Back Column Inl EPC PCM CH CAP () Column Col : 9009P-QO, HP-PLOT Q, 5m x 0.mm x 0um Col : 909P-MS4, HP-PLOT Molsieve, 0m x 0.mm x um Restrictor: , Deactivated Fused Silica Tubing, 0.7m x 0. mm R P S 888 Restrictor 0.7m x 0.mm Blank FSD Restrictor Tubing 6/86/ /XXX /XXX Options SP options Remarks, x0, 05, 06, 09, 70, 75, 860, 888 Bio-ethanol fermentation analysis.

24 System Operation: Sample Inject FLOW INJECTION OVEN LEFT SIDE SOURCE PORT = #87X 5/86/ Valve System Date : Order No : VALVE COMPARTMENT BLOCK BLOCK 4/XXX /XXX S/N : Item : DETECTOR. 5 4 LOOP 6 IN SAMPLE OUT Back Inl EPC PCM CH CAP () H, O, N, CH4, CO, CO, HC s Column Col : 9009P-QO, HP-PLOT Q, 5m x 0.mm x 0um Col : 909P-MS4, HP-PLOT Molsieve, 0m x 0.mm x um Restrictor: , Deactivated Fused Silica Tubing, 0.7m x 0. mm R P S 888 Column Restrictor 0.7m x 0.mm Blank FSD Restrictor Tubing 6/86/ /XXX /XXX Options SP options Remarks, x0, 05, 06, 09, 70, 75, 860, 888 Bio-ethanol fermentation analysis. 4

25 System Operation, Valve 0.8 min FLOW INJECTION OVEN LEFT SIDE SOURCE PORT = #87X 5/86/ Valve System Date : Order No : VALVE COMPARTMENT BLOCK BLOCK 4/XXX /XXX S/N : Item : DETECTOR. 5 4 LOOP 6 IN SAMPLE OUT Back Inl EPC PCM CH CAP () CO, HC s Column Col : 9009P-QO, HP-PLOT Q, 5m x 0.mm x 0um Col : 909P-MS4, HP-PLOT Molsieve, 0m x 0.mm x um Restrictor: , Deactivated Fused Silica Tubing, 0.7m x 0. mm R P S 888 Column H, O, N, CH4,CO, Restrictor 0.7m x 0.mm Blank FSD Restrictor Tubing 6/86/ /XXX /XXX Options SP options Remarks, x0, 05, 06, 09, 70, 75, 860, 888 Bio-ethanol fermentation analysis. 5

26 System Operation: Valve min FLOW INJECTION OVEN LEFT SIDE SOURCE PORT = #87X 5/86/ Valve System Date : Order No : VALVE COMPARTMENT BLOCK BLOCK 4/XXX /XXX S/N : Item : DETECTOR. 5 4 LOOP 6 IN SAMPLE OUT Back Inl EPC PCM CH CAP () Column Col : 9009P-QO, HP-PLOT Q, 5m x 0.mm x 0um Col : 909P-MS4, HP-PLOT Molsieve, 0m x 0.mm x um Restrictor: , Deactivated Fused Silica Tubing, 0.7m x 0. mm R P S 888 Column H, O, N, CH4,CO, CO, HC s Restrictor 0.7m x 0.mm Blank FSD Restrictor Tubing 6/86/ /XXX /XXX Options SP options Remarks, x0, 05, 06, 09, 70, 75, 860, 888 Bio-ethanol fermentation analysis. 6

27 Results PPQ Channel: CO, ethylene, ethane, HS, water, propane, and ethanol Molsieve Channel: H, O, N, CH4, CO 7

28 Molsieve Channel: H, O, N, CH4, CO 8

29 PPQ Channel: CO, ethylene, ethane, HS, water, propane, and ethanol 9

30 PPQ Channel: CO, ethylene, ethane, HS, water, propane, and ethanol 0

31 Flexible Configuration Easily modified to include additional channels and detectors FLOW INJECTION OVEN LEFT SIDE SOURCE PORT = #87X 5/86/ Valve System Date : Order No : VALVE COMPARTMENT BLOCK BLOCK 4/XXX /XXX S/N : Item : DETECTOR. 5 4 Back Aux AUX Back Inl EPC Inl EPC Back CAP () CAP () Column Column 4a LOOP R P 888 S Column 4b 6 Sample In Column Column Side () Back FID (0) Flexible Detector Choices: Options 6/86/ x, 0, 0,, 0, 05, 06, x70, 75, x860, 880, 888, 4xG , x588-56, G , , , , CP7554, 9095P- MS0E, -06, 5-5, 4xG /XXX SP options , LOOP Sample Out /XXX Remarks Column Info: Column : CP7554, PoraPLOT Q, 5m x0.5mm x 0um Column : 9095P-MS0E, 0m x 0.5mm x 50um Column : Restrictor, fused silica deactivated tubing Column 4a: -06, (5m cut), 60m x 0.5mm x.0 um Column 4b: -06, (55m cut), 60m x 0.5mm x.0 um FID MSD ECD FPD SCD NCD

32 GC Platforms 780 GC Entry Level Price/Performance LTM /7890 GC Fast heating/ cooling 490 Micro GC Fast Gas Analysis Compact Size 7890 GC Highest flexibility Industry leader Technologies 6850 GC Small footprint

33 Inlets and Detectors Introduced or refreshed in FY007-00

34 Thank You! Any Questions? 4