Scion 456-GC User manual

Reference Manual
CO/CO2 Analyzer
SCION Instruments HQ SCION Instruments NL BV
Suite 34, Livingston Business Centre, 4462, Goes,
Kirkton Road South, Livingston, Stanleyweg 4.
EH54 7FA, Scotland, UK. The Netherlands
Tel: [phone] Tel: [phone]
sales-[email protected] sales-[email protected]
www.scioninstruments.com www.scioninstruments.com
Revised February 2019
© 2015 Scion Instruments

SCION Instruments
Scion Instruments CO/CO2Analyzer Page 2
SECTION CONTENTS
INTRODUCTION...........................................................................................................3
INSTRUMENT SPECIFICATIONS ............................................................................4
INSTALLATION OF COLUMNS, FLOW AND PRESSURE SETTING ..............5
TUNING OF THE CO/CO2 CHANNEL.....................................................................6
OPERATION ..................................................................................................................9
TROUBLE SHOOTING.............................................................................................. 11
STEP BY STEP............................................................................................................ 12

Scion Instruments
Scion Instruments CO/CO2Analyzer Page 3
INTRODUCTION
The CO/CO2Analyzer Channel is an analytical tool principally developed for
the simultaneous determination of carbon monoxide, methane and carbon
dioxide in various gaseous hydrocarbon matrices or pure-gas samples.
The sample is injected by means of a gas-sampling valve onto a series of
Hayesep-R columns. The first fraction, containing the components of
interest is sent to a methanizer-FID combination; the rest of the sample is
backflushed.
The CO/CO2Analyzer Channel is set for the determination of the mentioned
components down to sub ppm levels.
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 CO/CO2Analyzer Page 4
INSTRUMENT SPECIFICATIONS
The instrument specifications are published in the corresponding Data
Sheet
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 CO/CO2Analyzer 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 of pressure settings have been changed. New
columns have to be preconditioned, prior to installation!
Tuning of the analyzer is only necessary in case new columns are installed or
after flow or pressure settings are changed.
Make sure, the instrument is connected to the minimum gas supply
pressures as indicated in the pre installation requirements (in section 2 of
this manual).
For more detailed information concerning the configuration of the
instrument, please, refer to the drawing section (section 6 of this manual).
The drawing also outlines the way the analyzer channel has been
incorporated into the gas chromatograph.
Regularly check and replace filters in order to maintain the quality of
the gas supply as described in the pre installation requirements.
Replacement columns:
SC15892: SS COLUMN HAYESEP R 2.6M. (pre-column)
SC15886: SS COLUMN HAYESEP R 1M. (analytical column)

Scion Instruments
Scion Instruments CO/CO2Analyzer Page 6
TUNING OF THE CO/CO2 CHANNEL
Connect the columns according the flow schematics given in Section 6
and adjust the flows (if necessary) at an oven temperature of 50°C.
Take very good care not to create any dead volume.
•Set the injection/backflush valve V1 to the inject (+) position.
•Disconnect both columns from the pressure point Tee and connect both
columns to each other using a 1/8” union.
•Set the front EFC-24 pressure to give a flow of 20 ml/min measured at the
FID outlet.
•Remove the 1/8 “union between the two columns and reconnect the
columns at the pressure point union Tee.
•Set the middle EFC-24 pressure to give a flow of 25 ml/min measured at the
FID outlet.
•Program for each EFC-24 module the total flow as mentioned in the
'OPERATION' paragraph.
•Adjust the Hydrogen Manual Flow Controller to give a flow of 20 ml/min
measured at the FID outlet (Note: total carrier plus Methanizer hydrogen is
45 ml/min)
•Set the injection/backflush valve to the load(-) position. Set the needle valve
NV-1 controlling the backflush flow to 20 ml/min, to be measured at vent 1.
Check all connections for leakages.
It is advised to use an electronic leak detector, since 'Snoop' or
equivalent soap solutions contaminate the analytical flowpath of
your instrument.

Scion Instruments
Scion Instruments CO/CO2Analyzer Page 7
The system is now ready for conditioning
Run the method continuously overnight to condition all columns.
Inject a reference sample, containing all relevant components, preferably in
helium or nitrogen. The result should look like Figure 1.
Set the backflush of the Hayesep columns to allow full recovery of the CO2.
Depending on the sample matrix, pure-gases or ethylene or propylene and
depending on the sample loop installed, the optimum backflush time may
be different. The optimum backflush time must be determined for the
individual matrices. See Figure 2 for trace determination of CO and CO2in
propylene.
Figure 1: CO/CO2analyzer example chromatogram (sample loop: 0.5 ml)
The individual concentrations are around 50 ppm in nitrogen.
Minutes
0
1
2
3
4
5
6
7
8
9
10
Vol
ts
0.005
0.010
0.015
0.020
0.025
0.030
Vol
ts
0.005
0.010
0.015
0.020
0.025
0.030
Detector 1
CO
CH4
CO2

Scion Instruments
Scion Instruments CO/CO2Analyzer Page 8
All factory tests are performed using helium as the carrier gas. However,
nitrogen or hydrogen may be used as the carrier gas. The choice depends
on the final application. If another gas as helium is the carrier gas, the
various detector flows as well as the method need to be adapted to the new
situation.
Figure 2: Example chromatogram of propylene matrix (sample loop: 5 ml)
The concentration of Carbonmonoxide is 100 ppb.
Minutes
1
2
3
4
5
6
7
8
9
Vol
ts
0.002
0.003
0.004
0.005
0.006
0.007
0.008
0.009
Vol
ts
0.002
0.003
0.004
0.005
0.006
0.007
0.008
0.009
Detector 1
CO
CH4
CO2

Scion Instruments
Scion Instruments CO/CO2Analyzer Page 9
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 (IBV)
V2 (S)
Initial
-
-
initial state
0.10
-
+
sample flush
0.80
-
-
sample flush (stop)
1.00
+
-
injection
4.50
-
-
backflush
Flow/Pressure
Front EFC-24 (He):
Pressure (PSI)
Hold (min)
Initial:
27.5
15
Total Flow: 50 ml/min
Middle EFC-24 (He):
Pressure (PSI) Hold (min)
Initial:
14.5
15
Total Flow: 50 ml/min
Column Oven:
Temp(ºC)
Rate(ºC/min)
Hold(min)
Total(min)
Initial
50
0
15.00
15.00
Valve Oven:
Temp: 100 (ºC)
Methanizer Oven:
Temp: 400 (ºC)
Flow (H2) 20 ml/min
Detector (Middle FID):
Temp: 200 (ºC)
Range: 12
Time Constant: slow
Front DEFC 11:
Air flow: 300 ml/min
H2: 10 ml/min
Make up: 15 ml/min N2

Scion Instruments
Scion Instruments CO/CO2Analyzer Page 10
This method is only valid in case the instrument is equipped with one
CO/CO2 Analyzer channel only. Refer to section 1 for the actual method(s),
whenever the instrument has combined channels.
Never interrupt an analytical run. The complete cycle has to finish.
The sample has to be connected to the 'sample in' at the right-hand side of
the instrument. The 'sample out' is preferably connected to a fume hood or
other exhaust.
At the beginning of the run, the sample loop is flushed for about 1 minute
(this is part of the method). Just before injection, the sample flow is stopped
to allow equilibration of the sample to atmospheric pressure.
In case there is a large difference in concentration between two consecutive
runs it is advised to allow for a pre-flush of the sample loops before starting
the automated run. This is done by manually activating the sample solenoid.

Scion Instruments
Scion Instruments CO/CO2Analyzer Page 11
TROUBLE SHOOTING
For problems related to the basic hardware and electronics of the gas
chromatograph, as well as injectors and detectors, refer to the 456-GC 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.
The presence of oxygen in the sample will influence the (accurate)
determination of carbon monoxide. This is due to the oxidation of deposited
carbon on the methanizer, and almost coëlution of oxygen and carbon
monoxide.
If a hydrocarbon gas, ethylene or propylene is the sample matrix, the
backflush time must be set to have maximum recovery for carbon dioxide in
combination with complete backflush of the matrix components. High
amounts of hydrocarbons will create excess deposition of carbon on the
methanizer column, reducing the methanizer lifetime.
Trace impurities of oxygen and carbon dioxide in the carrier gases, may
easily influence the determination at low levels. Increased noise levels will
have a negative influence on the limits of detection. Carefully follow the pre-
installation requirements concerning carrier gas purity and filter
requirements.
The methanizer needs to be replaced in case of:
•severe peak tailing for carbon monoxide and carbon dioxide
•variations in the conversion efficiency of the methanizer
•missing carbon monoxide and carbon dioxide.
CONSUMABLES
Partnumber Description
03-923720-31 Nickel catalyst column
03-911600-02 30 % Nickel Nitrate on Chrom PAW 100-120 mesh
SC15892 SS column Hayesep R2.6M
SC15886 SS column Hayesep R 1M
BRF0102 Super Clean™ Gas Filter OXYGEN
BRF0101 Super Clean™ Gas Filter MOISTURE

Scion Instruments
Scion Instruments CO/CO2Analyzer Page 12
STEP BY STEP
Step by step customer drawings CO/CO2Analyzer

Scion Instruments
Scion Instruments CO/CO2Analyzer Page 13
Fill position

Scion Instruments
Scion Instruments CO/CO2Analyzer Page 14
Inject position

Scion Instruments
Scion Instruments CO/CO2Analyzer Page 15
Backflush position