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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 17, 2012 1

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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 17, 2012

1

• Simplified design

• Easier setup

• Easier maintenance

• Capillary columns

• Faster chromatography

Advantages to Using Micro-fluidics for Analysis of

Permanent Gases in Various Matrices

2

Example: Bio-Ethanol Fermentation Monitoring

3

System Design: Picking Columns

4

5

J. Sep. Sci. 2008, 31, 3385 – 3394

But wait…

6

Deans Switch Heart-cutting 2-D GC provides extremely high chromatograpic

resolution

7

Cut

Deans

Switch

Auto- sampler

7890A GC

FID1 FID2

Column 1 Column 2

.

Back

Front

PCM

Front

TCD

(220)

TCD

(220)

(112)

CAP

Molesieve

HP PLOT Q

Restrictor

P

S

R1

3

PCM X

Ch 1

Ch 2 2

13

Deans Switch

8

Deans Switch

9

.

Back

Front

PCM

Front

TCD

(220)

TCD

(220)

(112)

CAP

Molesieve

HP PLOT Q

Restrictor

P

S

R1

3

2

13

PCM X

Ch 1

Ch 2

Deans Switch

10

.

Back

Front

PCM

Front

TCD

(220)

TCD

(220)

(112)

CAP

Molesieve

HP PLOT Q

Restrictor

P

S

R1

3

2

13

PCM X

Ch 1

Ch 2

• 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

System Design

11

.

Order No :

Date : 03-08-2012

Remarks

FLOW

SOURCE

INJECTION

PORT

VALVE COMPARTMENT

BLOCK 2 BLOCK 1DETECTOR

S/N :

Item :

Options

OVEN LEFT SIDE

Valve System

SP1 options

Back

Front

PCM

Front Inl Front

1/XXX

2/XXX3/XXX

4/XXX5/861/

6/861/

= #87X

TCD(220)

TCD

(220)

(112)

CAPEPC

12

3

4

5

6

IN

OUT

SAMPLE

LOOP

CH 1

Column 2

Column 1

Restrictor

0.37m x 0.1mm Blank FSD

Restrictor Tubing

Col 1: 190091P-QO3, HP-PLOT Q, 15m x 0.32mm x 20um

Col 2: 19091P-MS4, HP-PLOT Molsieve, 30m x 0.32mm x 12 um

Restrictor: 160-2255-30, Deactivated Fused Silica Tubing, 0.37m x 0.1 mm

888P

S

R1

3

21

3

112, 2x220, 305, 306, 309, 701, 751, 860, 888 Bio-ethanol fermentation analysis.

Valve Configuration

12

Column Configuration

13

Column 1 Flow

14

Column 2 Flow

15

Column 3 Flow

16

Setting the Heart Cut Time Start with Deans Switch Valve off

17

System Operation: Sample Load

18

.

Order No :

Date : 03-08-2012

Remarks

FLOW

SOURCE

INJECTION

PORT

VALVE COMPARTMENT

BLOCK 2 BLOCK 1DETECTOR

S/N :

Item :

Options

OVEN LEFT SIDE

Valve System

SP1 options

Back

Front

PCM

Front Inl Front

1/XXX

2/XXX3/XXX

4/XXX5/861/

6/861/

= #87X

TCD(220)

TCD

(220)

(112)

CAPEPC

12

3

4

5

6

IN

OUT

SAMPLE

LOOP

CH 1

Column 2

Column 1

Restrictor

0.37m x 0.1mm Blank FSD

Restrictor Tubing

Col 1: 190091P-QO3, HP-PLOT Q, 15m x 0.32mm x 20um

Col 2: 19091P-MS4, HP-PLOT Molsieve, 30m x 0.32mm x 12 um

Restrictor: 160-2255-30, Deactivated Fused Silica Tubing, 0.37m x 0.1 mm

888P

S

R1

3

21

3

112, 2x220, 305, 306, 309, 701, 751, 860, 888 Bio-ethanol fermentation analysis.

.

Order No :

Date : 03-08-2012

Remarks

FLOW

SOURCE

INJECTION

PORT

VALVE COMPARTMENT

BLOCK 2 BLOCK 1DETECTOR

S/N :

Item :

Options

OVEN LEFT SIDE

Valve System

SP1 options

Back

Front

PCM

Front Inl Front

1/XXX

2/XXX3/XXX

4/XXX5/861/

6/861/

= #87X

TCD(220)

TCD

(220)

(112)

CAPEPC

12

3

4

5

6

IN

OUT

SAMPLE

LOOP

CH 1

Column 2

Column 1

Restrictor

0.37m x 0.1mm Blank FSD

Restrictor Tubing

Col 1: 190091P-QO3, HP-PLOT Q, 15m x 0.32mm x 20um

Col 2: 19091P-MS4, HP-PLOT Molsieve, 30m x 0.32mm x 12 um

Restrictor: 160-2255-30, Deactivated Fused Silica Tubing, 0.37m x 0.1 mm

888P

S

R1

3

21

3

112, 2x220, 305, 306, 309, 701, 751, 860, 888 Bio-ethanol fermentation analysis.

System Operation: Sample Inject

19

H2, O2, N2, CH4,

CO, CO2, HC’s

.

Order No :

Date : 03-08-2012

Remarks

FLOW

SOURCE

INJECTION

PORT

VALVE COMPARTMENT

BLOCK 2 BLOCK 1DETECTOR

S/N :

Item :

Options

OVEN LEFT SIDE

Valve System

SP1 options

Back

Front

PCM

Front Inl Front

1/XXX

2/XXX3/XXX

4/XXX5/861/

6/861/

= #87X

TCD(220)

TCD

(220)

(112)

CAPEPC

12

3

4

5

6

IN

OUT

SAMPLE

LOOP

CH 1

Column 2

Column 1

Restrictor

0.37m x 0.1mm Blank FSD

Restrictor Tubing

Col 1: 190091P-QO3, HP-PLOT Q, 15m x 0.32mm x 20um

Col 2: 19091P-MS4, HP-PLOT Molsieve, 30m x 0.32mm x 12 um

Restrictor: 160-2255-30, Deactivated Fused Silica Tubing, 0.37m x 0.1 mm

888P

S

R1

3

21

3

112, 2x220, 305, 306, 309, 701, 751, 860, 888 Bio-ethanol fermentation analysis.

System Operation:

20

H2, O2, N2, CH4, CO,

CO2, HC’s

Valve 1 OFF

Finding the Cut Time for the Deans Switch Valve

21

Air

0.8 min

Valve 1 ON

1.2 min

Valve 1 OFF

Add Valves Times to Run Time Events Table

22

System Operation: Sample Load

23

.

Order No :

Date : 03-08-2012

Remarks

FLOW

SOURCE

INJECTION

PORT

VALVE COMPARTMENT

BLOCK 2 BLOCK 1DETECTOR

S/N :

Item :

Options

OVEN LEFT SIDE

Valve System

SP1 options

Back

Front

PCM

Front Inl Front

1/XXX

2/XXX3/XXX

4/XXX5/861/

6/861/

= #87X

TCD(220)

TCD

(220)

(112)

CAPEPC

12

3

4

5

6

IN

OUT

SAMPLE

LOOP

CH 1

Column 2

Column 1

Restrictor

0.37m x 0.1mm Blank FSD

Restrictor Tubing

Col 1: 190091P-QO3, HP-PLOT Q, 15m x 0.32mm x 20um

Col 2: 19091P-MS4, HP-PLOT Molsieve, 30m x 0.32mm x 12 um

Restrictor: 160-2255-30, Deactivated Fused Silica Tubing, 0.37m x 0.1 mm

888P

S

R1

3

21

3

112, 2x220, 305, 306, 309, 701, 751, 860, 888 Bio-ethanol fermentation analysis.

System Operation: Sample Inject

24

H2, O2, N2, CH4,

CO, CO2, HC’s

.

Order No :

Date : 03-08-2012

Remarks

FLOW

SOURCE

INJECTION

PORT

VALVE COMPARTMENT

BLOCK 2 BLOCK 1DETECTOR

S/N :

Item :

Options

OVEN LEFT SIDE

Valve System

SP1 options

Back

Front

PCM

Front Inl Front

1/XXX

2/XXX3/XXX

4/XXX5/861/

6/861/

= #87X

TCD(220)

TCD

(220)

(112)

CAPEPC

12

3

4

5

6

IN

OUT

SAMPLE

LOOP

CH 1

Column 2

Column 1

Restrictor

0.37m x 0.1mm Blank FSD

Restrictor Tubing

Col 1: 190091P-QO3, HP-PLOT Q, 15m x 0.32mm x 20um

Col 2: 19091P-MS4, HP-PLOT Molsieve, 30m x 0.32mm x 12 um

Restrictor: 160-2255-30, Deactivated Fused Silica Tubing, 0.37m x 0.1 mm

888P

S

R1

3

21

3

112, 2x220, 305, 306, 309, 701, 751, 860, 888 Bio-ethanol fermentation analysis.

.

Order No :

Date : 03-08-2012

Remarks

FLOW

SOURCE

INJECTION

PORT

VALVE COMPARTMENT

BLOCK 2 BLOCK 1DETECTOR

S/N :

Item :

Options

OVEN LEFT SIDE

Valve System

SP1 options

Back

Front

PCM

Front Inl Front

1/XXX

2/XXX3/XXX

4/XXX5/861/

6/861/

= #87X

TCD(220)

TCD

(220)

(112)

CAPEPC

12

3

4

5

6

IN

OUT

SAMPLE

LOOP

CH 1

Column 2

Column 1

Restrictor

0.37m x 0.1mm Blank FSD

Restrictor Tubing

Col 1: 190091P-QO3, HP-PLOT Q, 15m x 0.32mm x 20um

Col 2: 19091P-MS4, HP-PLOT Molsieve, 30m x 0.32mm x 12 um

Restrictor: 160-2255-30, Deactivated Fused Silica Tubing, 0.37m x 0.1 mm

888P

S

R1

3

21

3

112, 2x220, 305, 306, 309, 701, 751, 860, 888 Bio-ethanol fermentation analysis.

System Operation, Valve 1 ON @ 0.8 min

25

CO2, HC’s

H2, O2, N2, CH4,CO,

System Operation: Valve 1 OFF @ 1.2 min

26

CO2, HC’s

H2, O2, N2, CH4,CO,

.

Order No :

Date : 03-08-2012

Remarks

FLOW

SOURCE

INJECTION

PORT

VALVE COMPARTMENT

BLOCK 2 BLOCK 1DETECTOR

S/N :

Item :

Options

OVEN LEFT SIDE

Valve System

SP1 options

Back

Front

PCM

Front Inl Front

1/XXX

2/XXX3/XXX

4/XXX5/861/

6/861/

= #87X

TCD(220)

TCD

(220)

(112)

CAPEPC

12

3

4

5

6

IN

OUT

SAMPLE

LOOP

CH 1

Column 2

Column 1

Restrictor

0.37m x 0.1mm Blank FSD

Restrictor Tubing

Col 1: 190091P-QO3, HP-PLOT Q, 15m x 0.32mm x 20um

Col 2: 19091P-MS4, HP-PLOT Molsieve, 30m x 0.32mm x 12 um

Restrictor: 160-2255-30, Deactivated Fused Silica Tubing, 0.37m x 0.1 mm

888P

S

R1

3

21

3

112, 2x220, 305, 306, 309, 701, 751, 860, 888 Bio-ethanol fermentation analysis.

Results PPQ Channel: CO2, ethylene, ethane, H2S, water, propane, and ethanol

Molsieve Channel: H2, O2, N2, CH4, CO

27

Molsieve Channel: H2, O2, N2, CH4, CO

28

PPQ Channel: CO2, ethylene, ethane, H2S, water,

propane, and ethanol

29

PPQ Channel: CO2, ethylene, ethane, H2S, water,

propane, and ethanol

30

Flexible Configuration

31

.

Order No :

Date :

Remarks

FLOW

SOURCE

INJECTION

PORT

VALVE COMPARTMENT

BLOCK 2 BLOCK 1DETECTOR

S/N :

Item :

Options

OVEN LEFT SIDE

Valve System

SP1 options

Side

Back

Front Front Inl

Back Inl

Back Aux

Back

1/XXX

2/XXX3/XXX

4/XXX5/861/

6/861/

= #87X

TCD

FID

(220)

(210)

TCD

(221)

Front

(112)

CAP

(112)

CAPEPC

EPC

AUX 2

3

1

888P

S

R1

3

12

3

4

5

6

LOOP

12

3

4

5

6

LOOP

21

3

Column 1

Column 4a Column 4b

Column 2

Column 3

2x112, 210, 220, 221, 301, 305, 306, 2x701, 752, 2x860,

880, 888, 4xG2855-20530, 2x5188-5363, G2855-60200,

160-2255-30, 160-2325-30, 160-2615-10, CP7554, 19095P-

MS0E, 123-1036, 115-3352, 4xG2855-20590

7890-0990, 7890-0999

Column Info:

Column 1: CP7554, PoraPLOT Q, 25m x0.53mm x 20um

Column 2: 19095P-MS0E, 30m x 0.53mm x 50um

Column 3: Restrictor, fused silica deactivated tubing

Column 4a: 123-1036, (5m cut), 60m x 0.25mm x 1.0 um

Column 4b: 123-1036, (55m cut), 60m x 0.25mm x 1.0 um

Sample In

Sample Out

• Easily modified to include additional channels and detectors

Flexible

Detector

Choices:

FID

MSD

ECD

FPD

SCD

NCD

GC Platforms

32

7820 GC

Entry Level

Price/Performance

6850 GC

Small footprint

7890 GC

Highest flexibility

Industry leader

Technologies

LTM /7890 GC

Fast heating/

cooling

490 Micro GC

Fast Gas Analysis

Compact Size

Inlets and Detectors

33

Introduced or refreshed

in FY2007-2010

Thank You!

34

Any Questions?