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Scion Instruments 400-GC Series, 456-GC Reference guide

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Suite 34, Livingston Business Centre, 4462, Goes,
Kirkton Road South, Livingston, Stanleyweg 4.
EH54 7FA, Scotland, UK. The Netherlands
Tel: +44 1506 300 200 Tel: +31 113 348 926
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www.scioninstruments.com www.scioninstruments.com
Revised March 2019
© 2015 Scion Instruments
Reference Manual
Natgas C Analyzer
With Additional He/H
2
Channel
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 2
Section contents
INTRODUCTION .................................................................................................................................. 3
INSTRUMENT SPECIFICATIONS ................................................................................................... 4
INSTALLATION OF COLUMNS, FLOW AND PRESSURE SETTING ...................................... 5
TUNING THE NATGAS C ANALYZER ........................................................................................... 6
OPERATION ......................................................................................................................................... 7
TROUBLE SHOOTING ........................................................................................................................ 9
STEP BY STEP................................................................................................................................... 11
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 3
INTRODUCTION
Natural gas analysis commonly involves the quantitation of components up
to C5 while C6 and heavier hydrocarbons are combined and measured as a
single peak (C6+). Extending the analysis to obtain the compositional
breakdown of the C6+ group can provide valuable information.
The Natgas C Analyzer is an analytical tool principally developed for the
determination of oxygen, nitrogen, carbon dioxide, and the hydrocarbons C1
to C12. Three columns are used to accomplish the single-channel analysis of
natural gas: First a molecular sieve column for oxygen and nitrogen
separation, then a Hayesep P column for the separation of methane till
hydrogen sulfide and a capillary column for the separation of C1-C12
hydrocarbons.
The instrument is tuned during Final Test to its proper settings.
Do not change any flow or pressure settings unless it is
requested.
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 4
INSTRUMENT SPECIFICATIONS
Every instrument is fully tested; the results of the tests, as well as the
methods used during these tests, are presented as part of this manual (refer
to section 1).
START UP
At initial START-UP as well as after a longer idle period,
follow the instructions below:
• Connect all the gases to the instrument.
• Switch the power on.
• Load the appropriate method.
• Check the flow settings.
• Condition the system as described in this manual.
• Do not make any changes to the methods.
• The system is ready for injections.
For a new system there is no need to do any flow measurement or
flow tuning before power-up. The instrument is tuned and tested in
our Factory in Goes.
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 5
INSTALLATION OF COLUMNS, FLOW AND PRESSURE SETTING
Tuning of the analyzer is only necessary in case new columns are
installed or after flow or pressure settings have been changed.
Before new columns may be installed, they need to be
preconditioned!!
Make sure, the instrument is connected to the minimum gas supply
pressures as indicated in the 400-GC series pre-installation manual.
For more detailed information concerning the configuration of the
instrument, please, refer to the drawing section (section 6 of this manual).
The factory drawing indicates which flow and pressure controls are being
used. The drawing also outlines the way the analyzer channel has been
incorporated into the gas chromatograph.
Regularly check and replace filters maintaining the supply quality as
described in the pre installation requirements.
Replacement columns
SC30128 SCION-1, 60m x 0.25mm, df = 1.0 µm
SC15919 Molsieve 13X, 4ft * 1/8", Inert Steel
SC15922 Empty delay, 10 ft * 1/8", Inert Steel
SC15920 Hayesep P, 6 ft * 1/8", Inert Steel
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 6
TUNING THE NATGAS C ANALYZER
Tuning is only necessary when new columns have to be installed or by
malfunctioning of the GC.
Connect the columns according the flow schematics given in Section 6 and
adjust the pressures (if necessary) at an oven temperature of 45°C.
Take very good care not to create any dead volume!
• Set the injection valve (V1) and the column selection valve (V2) in the (-)
position.
• While measuring the flow out the exit of the middle TCD, adjust the rear
EFC-24 flow until there is a flow of 33 ml/min.
• Set the middle EFC-24 until a flow of 27 ml/min is coming out of the vent 1.
• Set the DEFC-13 to give a flow of 30 ml/min out of the reference exit of the
TCD.
• Set the front EFC-25 pressure at 20 psi and at a split ratio of 1:200.
• Program the method as given in the OPERATION section.
• Check all connections for leakage.
After stabilization of the TCD and FID signals the system is ready for
analyses.
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 7
OPERATION
An operational method is preloaded in the instrument.
Listed below is an example method; settings determining the application
may be different.
Sample delivery
V1 (GSV)
V2 (CS)
V4 (S)
Initial
-
-
-
0.01
- - +
0.80
-
-
-
1.00
+
-
-
1.91
+ + -
Injector (S/SL Front):
Temp 220 ºC
Split ratio 200
Flow/Pressure:
Front EFC-25:
Pressure (PSI)
Hold (min)
20.0
18.00
Middle EFC-24:
Pressure (PSI)
Hold (min)
14.0
18.00
Total Flow: 60 ml/min
Rear EFC-24:
Pressure (PSI)
Hold (min)
12.0
18.00
Total Flow: 60 ml/min
Column Oven:
Temp(ºC)
Rate(ºC/min)
Hold(min)
Total(min)
Initial
45
--
6.00
6.00
190
20
4.75
18.00
Oven stabilization time 0.50 minutes
The temperature is raised after elution of H
2
S.
Large Valve Oven:
Temp 100 ºC
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 8
Detector (middle TCD):
Temp 200 ºC
Range 0.05
Time constant slow
Fila temp: 230 °C
Fila max: 390 °C
Polarity: negative
Autozero: yes
DEFC-13
Reference: 30 ml/min
Detector (middle FID)
Temp: 300°C
Time constant: Slow
Range : 12
Autozero: No
DEFC-11
Make-up: 30 ml/min
Hydrogen: 30 ml/min
Air 300 ml/min
Never interrupt an analytical run. The complete cycle has to
finish!
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 9
TROUBLE SHOOTING
For problems related to the basic hardware and electronics of the gas
chromatograph, as well as injectors and detectors, refer to the 400-GC
Series user manual.
In case of any analytical problem, it is always advised to record an analysis
using a reference sample. The result, including full details can be submitted
to your local Scion Instruments service department to judge performance.
Fig. 1 and fig. 2 show chromatograms of the TCD and FID tracks respectively.
In case of decreasing retention times of the Molecular Sieve column, this
column needs reconditioning. This has to be done in a different oven under
nitrogen or helium at 350° C overnight.
Check the status of the humidity filter in case of conditioning is needed. The
cause might be saturation of this filter.
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 10
87.576.565.554.543.532.521.510.5
650,000
600,000
550,000
500,000
450,000
400,000
350,000
300,000
250,000
200,000
150,000
100,000
50,000
0
-50,000
O2/Ar
N2
O2/Ar/N2
CH4
CO2
C2H6
H2S
RT [min]
GC0903B101_NGA-C_5_5_2009 1_02_00 PM_1_28.DATA [Middle (TCD)]
µV
Fig 1: TCD channel
1817161514131211109876543210
1,400,000
1,300,000
1,200,000
1,100,000
1,000,000
900,000
800,000
700,000
600,000
500,000
400,000
300,000
200,000
100,000
0
CH4
C2H6
C3H8
i-C4H10
n-C4H10
i-C5H12
n-C5H12
n-C6H14
RT [min]
GC0903B101_NGA-C_5_5_2009 1_02_00 PM_1_28.DATA [Rear (FID)]
µV
Fig 2: FID channel
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 11
STEP BY STEP
Step by step customer drawings Natgas C Analyzer
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 12
Initial Position
EFC-24
rear
Helium
Gas sample IN
Gas sample OUT
(To HeH2 channel)
Sample loop 250 µL
Sample loop 250 µL
Sample loop 250 µL
FID
DEFC-11
rear
TCD
DEFC-13
middle
SCION-1
SC30128
Molsieve 13X
SC15919
Empty Delay column
SC15922
Hayesep P
SC15920
Vent 1
Liquid sample IN
Liquid sample OUT
EFC-25
front
Helium
EFC-24
middle
Helium
V-4
P
C
S
W
W
S
LSV 5
C
P
1
2
3
4
5
6
7
8
9
10
11
12
14
13
V - 1
1
2
3
4
5
6
V - 2
Reference TCD
Helium
S/SL Injector
front
Splitvent
Permanent gases channel
Hydrocarbons C1-C16 channel
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 13
Fill position
EFC-24
rear
Helium
Gas sample IN
Gas sample OUT
(To HeH2 channel)
Sample loop 250 µL
Sample loop 250 µL
Sample loop 250 µL
FID
DEFC-11
rear
TCD
DEFC-13
middle
SCION-1
SC30128
Molsieve 13X
SC15919
Empty Delay column
SC15922
Hayesep P
SC15920
Vent 1
Liquid sample IN
Liquid sample OUT
EFC-25
front
Helium
EFC-24
middle
Helium
V-4
P
C
S
W
W
S
LSV 5
C
P
1
2
3
4
5
6
7
8
9
10
11
12
14
13
V - 1
1
2
3
4
5
6
V - 2
Reference TCD
Helium
S/SL Injector
front
Splitvent
FILL MODE V-1 (-) V-2 (-)
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 14
Inject position
EFC-24
rear
Helium
Gas sample IN
Gas sample OUT
(To HeH2 channel)
Sample loop 250 µL
Sample loop 250 µL
Sample loop 250 µL
FID
DEFC-11
rear
TCD
DEFC-13
middle
SCION-1
SC30128
Molsieve 13X
SC15919
Empty Delay column
SC15922
Hayesep P
SC15920
Vent 1
Liquid sample IN
Liquid sample OUT
EFC-25
front
Helium
EFC-24
middle
Helium
V-4
P
C
S
W
W
S
LSV 5
C
P
1
2
3
4
5
6
7
8
9
10
11
12
14
13
V - 1
1
2
3
4
5
6
V - 2
Reference TCD
Helium
S/SL Injector
front
Splitvent
INJECT MODE V-1 (+) V-2 (-)
FOREFLUSH
Scion Instruments
Scion Instruments Natgas C Analyzer +He/H
2
Channel Reference Manual Page: 15
Backflush position
EFC-24
rear
Helium
Gas sample IN
Gas sample OUT
(To HeH2 channel)
Sample loop 250 µL
Sample loop 250 µL
Sample loop 250 µL
TCD
DEFC-13
middle
SCION-1
SC30128
Molsieve 13X
SC15919
Empty Delay column
SC15922
Hayesep P
SC15920
Vent 1
Liquid sample IN
Liquid sample OUT
EFC-25
front
Helium
EFC-24
middle
Helium
V-4
P
C
S
W
W
S
LSV 5
C
P
1
2
3
4
5
6
7
8
9
10
11
12
14
13
V - 1
1
2
3
4
5
6
V - 2
Reference TCD
Helium
S/SL Injector
front
Splitvent
BACKFLUSH MODE V-1 (-) V-2 (+)
BACKFLUSH
FID
DEFC-11
rear
/