Advancements in Gas Chromatography Analyzers

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Transcript Advancements in Gas Chromatography Analyzers

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
Col 2
Col 5
Back Aux
Ch 2
PCM C
Ch 1
Back Inl
7 6 5
Out
Sample
4
8
4
9
10
3
1
2
Col 4
6
Vent
LOOP
7 6 5
3
5
2
Sample
1
In
4
8
9
10
Col 1
3
2
1
In
Loop
25ul
100 ul
TCD
Loop
(221)
250 ul
Back
Ch 2
PCM B
Ch 1
Front Inl
EPC
Side
Vent
TCD
(220)
Front
860 CAP
(112)
874
Col 6
FID
(210)
3
6
Col 3
4
4
5
The design looks complicated, but it
is really just three separate channels.
Each channel by itself is very simple.
Lets break it down.
Front
Col 8
2
3
5
6
2
1
1
Col 7
Agilent Fast Refinery Gas Analyzer
Utilizes Four Types of Rotary Valves
4
- Valves are always
depicted in the OFF
position unless otherwise
noted
Out
6
LOOP
7 6 5
3
5
2
1
Sample
4
8
9
10
3
2
1
Vent
In
IN
SAMPLE
OUT
Loop
6-port GSV (Opt 701)
10-port GSV with precolumn back-flush to
vent (Opt 801)
4
4
3
5
6
2
1
6-port column isolation
valve (Opt 702)
3
5
6
2
1
6-port sequence reversal
with pre-column back-flush
to detector (Opt 708)
Agilent 7890-0322 Fast Refinery Gas System
Three Gas Sample Valve Loops in Series
Hydrogen Channel
Hydrocarbon
Channel
7 6 5
Out
Sample
4
8
4
9
10
3
1
2
Permanent Gas
Channel
6
LOOP
7 6 5
3
5
2
1
4
8
Sample
9
10
3
1
2
In
Loop
100 ul
25ul
Loop
250 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.
Agilent 7890-0322 Fast Refinery Gas System
Hydrogen Analysis:
Back-flush
MolSieve
Ch 2
PCM C
Ch 1
4
8
Sample
Out
9
10
Loop
100 ul
3
1
2
Vent
Hayesep Q
7 6 5
Back Aux
Sample In
Side
TCD
(221)
• 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
Unibead
7 6 5
4
8
9
10
Unibead
Sample In
3
2
Vent
Sample
Out
1
Loop
Back Inl
250 ul
Back
Ch 2
PCM B
Ch 1
TCD
(220)
MolSieve
4
3
5
6
2
1
Agilent 7890-0322 Fast Refinery Gas System
Hydrocarbon Analysis
4
3
5
6
2
LOOP
1
25ul
Front Inl
EPC
Front
860 CAP
(112)
Front
2M 5um DB-1
874
FID
(210)
4
3
5
6
2
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
Order No : Universal NGA Item :
INJECTION
FLOW
SOURCE
OVEN LEFT SIDE
PORT
VALVE COMPARTMENT
BLOCK 1
BLOCK 2
5/852/861
= #87X
4/XXX
S
1/800/502/504
P
W
DETECTOR
Sample In
IN
SAMPLE
S/N :
Date : 2/5/2012
Valve System
C
Sample Out
7 6 5
1.0 mL
Loop
4
8
9
10
3
1
2
0.25 mL
Loop
Col 2
Back
R
Col 1
7890-0020 CAP
(112)
EPC
1
P
S
2
0.53mm FSOT
transfer line
888
Back
Col 3
3
3
Front
860 CAP
(112)
EPC
TCD
(220)
Col 4
1
Front Inl
G3184-60065
Back Inl
Front
4
874
5
6
3
FID
2
(210)
1
Front Aux SAMPLE
S
W
1
AUX 2
3
OUT
P
Col 5
C
0.25mm x 5m FSOT
transfer line
6/850/861
Options
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
3/XXX
Remarks
SP1 options
7890-0990,
7890-0020,
7890-0999
2/708/5x872
Col 1: HP-PLOT Q PT, 19095P-QO4PT, 30m x 0.53mm x 40um
Col 2: HP-PLOT Molsieve, 19095P-MS0E, 30m x 0.53mm x 30 um
Col 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 um
Col 5: DB-1, 123-1036, (58m cut), 60m x 0.25mm x 1.0 um
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
In Summery
Capillary Flow Technology
-- solves difficult application
problems easily & opens up
many new (and old)
possibilities for GC & GC/MS
36
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July 17, 2015