Advancements in Gas Chromatography Analyzers - Keeping up with New Technology

Chuck Runkle Gas Phase Product Specialist ASTS June 2013

Capillary Flow Technology -- solves difficult application problems easily & opens up many new (and old) possibilities for GC & GC/MS

– Column connections (connect pre-column) – Change MSD columns (without venting) – Backflush (Reverse flow through column) – Deans switch (heart cut select peaks to 2nd column) – Detector splitter (effluent split to two or more detectors) – Merge flows (2 columns to 1 MSD) – Comprehensive 2-D GC (cut all peaks to 2nd column) – etc.

Purged Ultimate Union

Agilent 7890-0322 Fast Refinery Gas Analyzer What is a Fast Refinery Gas Analyzer • 7890 GC is designed to analyze refinery gas in under 6 min. • The system has 5 valves and three detectors. • The FID is for measuring hydrocarbons from C1 to C5 while C6/C6+

components are back-flushed and measured as a single peak at the beginning of the analysis.

• The first TCD is configured with helium carrier gas to analyze permanent gases (CO2, CO, O2, N2).

• The second TCD is configured with nitrogen carrier gas to analyze hydrogen. This detector is mounted on the side of the instrument.

Agilent 7890-0322 Fast Refinery Gas System Three Channel System for Analysis of Hydrogen, Permanent Gases and Hydrocarbon Analysis

Side

Back

Front Front Inl

Back Inl

Back Aux

TCD

FID

(220)

(210)

TCD(221)

Front

(112)CAPEPC

PCM CCh 1

Ch 2

PCM BCh 1

Ch 2

1 23

4567

8

910Sample

In

Out

Loop

Vent 12

34

5

6LOOP

860 874

1 23

4567

8

910Sample

In

Loop

Vent

12

34

5

61

2

34

5

6

Col 1

Col 2

Col 3

Col 4

Col 5

Col 6

Col 7

Col 8

25ul250 ul100 ul

The design looks complicated, but it is really just three separate channels. Each channel by itself is very simple. Lets break it down.

Agilent Fast Refinery Gas Analyzer Utilizes Four Types of Rotary Valves

12

34

5

6

IN

OUTSAMPLE

LOOP

12

34

5

61

2

34

5

6

1 23

4567

8

910Sample

In

Out

Loop

Vent

6-port GSV (Opt 701) 10-port GSV with pre-column back-flush to

vent (Opt 801)

6-port column isolation valve (Opt 702)

6-port sequence reversal with pre-column back-flush

to detector (Opt 708)

- Valves are always depicted in the OFF position unless otherwise noted

Agilent 7890-0322 Fast Refinery Gas System Three Gas Sample Valve Loops in Series

1 23

4567

8

910Sample

Out

Loop

12

34

5

6LOOP

1 23

4567

8

910Sample

In

Loop25ul250 ul100 ul

• There are three gas sample valves, one for each channel. • Sample flows in through a single 1/16” tube and fills the gas sample loop

for each valve before injection. • All three channels are injected simultaneously. • All channels analyze in parallel after injection.

Hydrogen Channel Permanent Gas Channel

Hydrocarbon Channel

Agilent 7890-0322 Fast Refinery Gas System Hydrogen Analysis: Back-flush

Side

Back Aux

TCD(221)

PCM CCh 1

Ch 21 2

3

4567

8

910

Loop

Vent

100 ul

Hayesep Q

MolSieve

Sample In

Sample Out

• The valve is turned to the OFF position after hydrogen has eluted to the Molsieve column.

• Hydrogen is separated from helium on the MolSieve and analyzed on the TCD

• All permanent gases and hydrocarbons are back-flushed from the Hayesep column to vent.

Agilent 7890-0322 Fast Refinery Gas System Permanent Gas Analysis: Sample Load

BackBack Inl

TCD(220)

PCM BCh 1

Ch 2

1 23

4567

8

910

Loop

Vent

12

34

5

6

250 ul

Unibead

Unibead

MolSieve

Sample In

Sample Out

Agilent 7890-0322 Fast Refinery Gas System Hydrocarbon Analysis

Front Front Inl

FID(210)

Front

(112)CAPEPC

12

34

5

6LOOP

860 874

12

34

5

6

25ul

2M 5um DB-1

25M 8um HP-AL/S

Agilent Fast Refinery Gas Analyzer 3 Channels of Data in under 6 minutes

FID: Hydrocarbons

TCD1: Permanent Gases

TCD2: Hydrogen

Refinery Gas TCD

Universal Capillary Nat Gas Solution Value to Customers Features of the Universal Nat Gas Solution

• Can be configured with both LSV and GSV for both liquid and gas injections • The FID channel is configured with a 6-port backflush valve and a DB-1 60m x

0.25mm x 1.0um – This channel can be configured for either a C6+ backflush or an extended

analysis simply through a method change. • TCD channel is equipped with a Deans Switch configured with a PLOT Q capillary

column and a Molsieve column. The columns from the Deans Switch are teed into a single TCD to give a more compact analysis. – This channel can be configured to either separate oxygen and nitrogen or to

report a N2/O2 composite, simply through a method change. • H2S can be analyzed on the PLOT Q TCD channel.

– If the user needs high level H2S the system could be ordered with Hastelloy valves and Nickel tubing.

Simplified Natural Gas O2/N2 Composite

Natural Gas C6 Plus with O2 & N2

Natural Gas Extended with O2 & N2

Universal Capillary Nat Gas Solution Review Value to Customers • We currently have 15 natural gas analyzers • These systems all revolve around a matrix of 5 variables

– Extended Analysis – Hydrogen Capacity – O2/N2 separation – High H2S – Liquefied Samples

• We have the ability to configure one instrument based on CFT that can be configured around 4 of the 5 nat gas variables. This system will not analyze for hydrogen.

• We do not see a big need for hydrogen analysis in the nat gas industry and if a customer needs this, they can order a refinery gas system.

Universal Capillary Nat Gas Solution

860

Order No : Universal NGA

Date : 2/5/2012

Remarks

FLOWSOURCE

INJECTIONPORT

VALVE COMPARTMENT

BLOCK 2 BLOCK 1DETECTOR

S/N :

Item :

Options

OVEN LEFT SIDE

Valve System

SP1 options

Back Inl Back

1/800/502/504

2/708/5x8723/XXX

4/XXX5/852/861

6/850/861

= #87X

Front

(112)CAP

(112)CAPEPC

Front

FID(210)

Front Aux

Front Inl

EPC

7890-0990,7890-0020,7890-0999

2x112, 210, 220, 301, 305, 306, 502, 504, 708, 752, 800, 850, 852 860, 2x861, 5x872, 874, 888, 19095P-QO4PT, 19095P-MS0E,

160-2255-10, 123-1036, 160-2535-5

Col 1: HP-PLOT Q PT, 19095P-QO4PT, 30m x 0.53mm x 40umCol 2: HP-PLOT Molsieve, 19095P-MS0E, 30m x 0.53mm x 30 umCol 3: Restrictor, FST, 160-2255-10, (cut to 1.5m), 5m x 0.250mm Col 4: DB-1, 123-1036, (2m cut), 60m x 0.25mm x 1.0 umCol 5: DB-1, 123-1036, (58m cut), 60m x 0.25mm x 1.0 um

AUX 23

1

Col 1

Col 2

1 23

4567

8

910

1.0 mLLoop

0.25 mLLoop

Sample In Sample Out

7890-0020 888P

S

R 1

3

21

3

Back

TCD(220)

Col 3

12

34

5

6

Col 5

Col 4

874

CWPS

INSAMPLE

CWPS

OUT

SAMPLE

G31

84-6

0065

0.53mm FSOT transfer line

0.25mm x 5m FSOT transfer line

Universal Capillary Nat Gas Solution Example Chromatogram from TCD Channel

Universal Capillary Nat Gas Solution Review Example Chromatogram from FID Channel 79% Hexanes LPG Injection, Extended Analysis

MS with Fixed Gases

MS with Fixed Gases Single TCD

Capillary Flow Technology -- solves difficult application problems easily & opens up many new (and old) possibilities for GC & GC/MS

In Summery

July 30, 2013 Confidentiality Label

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