“Analyzer for the determination of Hydrocarbons

and Hydrogen”

Dedicated Instruction Manual

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“Analyzer for the determination of the Hydrocarbons and Hydrogen”
TRACE™ GC Ultra Dedicated Instruction Manual

May 2004 Edition

© 2003 Thermo Electron Italia S.p.A. All rights reserved.
Printed in Italy

Published by Thermo Electron Italia S.p.A., Strada Rivoltana, 20090 Rodano - Milan – Italy
Tel: +39 02 95059373 Fax: +39 02 95059388

Disclaimer Technical Information contained in this publication is for reference purposes only and is subject to change
without notice. Every effort has been made to supply complete and accurate information; however, Thermo Electron
assumes no responsibility and will not be liable for any errors, omissions, damage, or loss that might result from any use of
this manual or the information contained therein (even if this information is properly followed and problems still arise).

This publication is not part of the Agreement of Sale between Thermo Electron and the purchaser of a TRACE™ GC Ultra
system. In the event of any conflict between the provisions of this document and those contained in Thermo Electron’s
Terms and Conditions, the provisions of the Terms and Conditions shall govern.

Reference to System Configurations and Specifications supercede all previous information and are subject to change
without notice.

Trademarks
TRACE™ is a trademark of Thermo Electron Italia S.p.A. Other brand and product names may be trademarks or registered
trademarks of their respective companies.

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 Declaration

Manufacturer: Thermo Electron Italia S.p.A.

Thermo ElectronItalia S.p.A. is the manufacturer of the instrument described in this manual
and, as such, is responsible for the instrument safety, reliability and performance only if:
•installation
•re-calibration
•changes and repairs

have been carried out by authorized personnel and if:

•the local installation complies with local law regulations
•the instrument is used according to the instructions provided and if its operation is only
entrusted to qualified trained personnel

Thermo Electron Italia S.p.A. is not liable for any damages derived from the non-compliance
with the aforementioned recommendations.

Thermo Electron Italia S.p.A.

Strada Rivoltana
20090 RODANO (MI)

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S/N 20044223 4
 Index
Analyzer for the determination of the Hydrocarbons and Hydrogen……………………………

General Description 08
Description of the Analyzer 08
Analytical Unit 09
General Description 09
Valve Oven 09
Valve Functions 10
Set-up of Analyzer 11
Packed Column Conditioning 11
Nuts Tightening 11
Leak Check Hydrogen Channel 11
Leak Check Hydrocarbons Channel 12
Analytical Tuning 13
Analytical Separation Hydrogen Channel 14
Analytical Separation Hydrocarbons Channel 14
Analytical Parameters 15
Analytical Result 16
Troubleshooting 18
Loss of chromatographic solution 18
Increase of the Height of interfering Peaks 18
Consumables 18

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Analyzer for the determination of the
Hydrocarbons and Hydrogen

This manual describes detailed operation of a dedicated GC configuration based on the

TRACE GC Ultra gas chromatograph and manufactured by Thermo Milan, equipped with
one TCD (Thermal Conductivity Detector) and one FID (Flame Ionization Detector) able
to perform the analysis of Hydrocarbons and Hydrogen.

Index…
General description 08
Analytical Unit 09
Set-up of analyzer 11
Analytical tuning 13
Analytical result 16
Troubleshooting 18
Consumables 18

For typographical conventions, symbols and customer communication please refer to

Operating Manual of the TRACE GC Ultra.

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General Description
Description of the Analyzer
The Trace GC Ultra is equipped with a Valve Oven housing, which includes two zones, a
heated and a cold one. In the heated area of the Valve Oven are installed two valves and
packed columns. The capillary column is installed inside the GC Oven.
Valve #2, gas sampling valve, also permits to backflush the packed columns for a quicker
elution to vent of remaining components.
Valve #3, gas sampling valve, make the injection on the Hydrocarbons Channel.
The complete configuration of the system is shown in the figure1-1.

Figure 1-1 Configuration of the system

Legend Description
Carrier 1 Left Carrier Gas (Helium) Hydrocarbons Channel
CG1 Manual Carrier Gas (Nitrogen) Hydrogen Channel
CG2 Manual Carrier Gas (Nitrogen) Hydrogen Channel
NV1 Needle Valve which can be used to adjust the carrier flow for TCD.
Regulation of this valve can be accomplished from the front part of
the valve oven.
NV2 Needle Valve which can be used to set a back pressure on the
sample loop for Hydrogen channel. Regulation of this valve can be
accomplished from the front part of the valve oven.
NV3 Needle Valve which can be used to set a back pressure on the
sample loop for Hydrocarbons channel. Regulation of this valve can
be accomplished from the front part of the valve oven.
In/Out Hydrogen Sample In – Sample Out in the front of Valve Oven for Hydrogen
Channel
In/Out Hydrocarbons Sample In – Sample Out in the front of Valve Oven for
Hydrocarbons Channel

Never close completely the needle valves otherwise the valve needle could be
irreversible damage.

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Analytical Unit

General Description
The system includes the following analytical channels:

Hydrocarbons Channel
This channel includes one capillary column:
- 50 m, 0.53 ID RT-Alumina, 6 µm film thickness.
The sample is injected by Valve # 3, with 250 µl sample loop.

Hydrogen Channel
The system include the following packed columns:
- Column 1: 1 m, 1/8” Molecular Sieve 13X, 60 - 80 mesh.
- Column 2: 1 m, 1/8” Haysep Q, 60 - 80mesh.
The sample is introduced by valve # 2, with 1 ml sample loop.

The analysis of Hydrocarbons and hydrogen are described following in detail.

Valve Oven
The Valve Oven temperature can be programmed between 40°C up to 175°C in the Aux
page of the TRACE GC. In order to heat the valve oven use the following steps:
- On the TRACE GC keypad press AUX button
- Scroll to Temperature Zones and press ENTER button
- Enter the target temperature and press ENTER button.

The Valve switching is controlled through the VALVE interface page on the TRACE GC
keypad and may be manually actuated by pressing ON/OFF buttons on the keypad or time
programmed through the RUN TIME menu on the Trace GC keyboard.
Manual switching of the valve is useful for set-up the analyzer step by step, or for
troubleshooting.

In order to switch the valve manually use the following steps (for instance for valve #1):
- Press VALVES button on the TRACE GC keypad
- Select gas sample valve #1
- Press ON to place the valve in the inject position or OFF to place the valve in the
load position.

The switching of all valves has been factory set-up in the RUN TABLE menu. You can
change the switching time of these valves by adding the desired value to the RUN TABLE.
The following steps allow you to change these values (for instance for valve #1):
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 - On the TRACE GC keypad press the RUN TABLE button
- Scroll to Add Run Time Event and press ENTER button
- Select Valve and press ENTER
- Scroll to Sampling valve #1 and press ENTER

The following screen appears:

o Inject at parameter is the time into the run that the sample is to be injected.
o Inject for parameter is the time that the valve will be returned to the Load position.

If the Inject for time exceeds the GC run time, the GC will automatically reset the valve to
the Load position at the end of the run.

Valve Functions

Valve# Setting Function

Valve# 2 Load Fill 1 ml sample loop and backflush the packed columns
Valve# 2 Inject for Inject on analytical channel
Valve# 3 Load Fill 250 µl sample loop for Hydrocarbons columns
Valve# 3 Inject for Inject on analytical channel

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Set-up of Analyzer
The analyzer is supplied fully tested for the specific analysis and it is equipped with
dedicated columns. However, during the transportation, vibrations and thermal fluctuations
could loose some nuts. Additionally some air can diffuse and be adsorbed on to the column.
The following procedure must be therefore applied in order to get smooth installation of the
instrument in the lab.

Packed Columns Conditioning

All columns must be conditioned before operating. Because of the different nature of their
stationary phases these have to be conditioned at different temperatures and therefore in
different steps.
o Haysep column must NOT exceed 180°C during conditioning
o Molecular Sieve column must NOT exceed 300°C during conditioning
o Capillary column must NOT exceed 200°C during conditioning
We strongly recommend to condition all these columns in an external Oven at a temperature
10°C lower than the maximum indicated above at a carrier gas flow rate of (suggested He)
20 ml/min for packed columns and 5 ml/min for capillary column. Columns conditioning
should be performed for at least four hours.

Nuts Tightening
Control all the nuts present in the column oven and in the heated Valve Oven and
tighten them if needed, paying attention not to over-tighten them with an
excessive strength.

Leak check on Hydrogen Gas channel

To perform a leak check, operate as follows:

1. Connect the columns and all the gases to the back of the Valve Oven.
2. Place the Valve #2 in the Inject position.
3. Cap the Right TCD detector outlet at the top of the GC by using a stopper and Cap
the vent outlet
4. Set the pressure of the GC1 and GC2 at value of 100 kPa. Maintain the system in
this condition for at least two minutes.
5. Close the manual regulators. Observe for any pressure decrease in the pressure
gauge in the next two minutes. If the pressure does not decrease this means that the
system is leak free.
6. In case of leak try to identify the leak point repeating the above operations and
checking all connections starting from the valve. If the system is leak free, place the
Valve #2 in the Load position and repeat steps 4 and 5.
7. Remove the cap.

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Leak check on Hydrocarbons channel
To perform a leak check, operate as follows:

1.Connect the column and all the gases to the back of the GC.
2.Place the Valve #3 in the Inject position.
3. Cap the Fid base body using the blind jet p/n 40401901 provided in the standard
outfit. Turn off the split and septum purge vents of the split/splitless injector
4.Set the pressure of the Left DPFC at a value of 100 kPa. Maintain the system in this
condition for at least two minutes.
5. Set the carrier Off and observe for any pressure decrease in the display in the
next two minutes. If the pressure does not decrease this means that the system
is leak free.
6. In case of leak try to identify the leak point repeating the above operations and
checking all connections starting from the valve. A leak tester will also help in this
operation. If the system is leak free place the Valve #3 in the Load position and repeat
steps 4 and 6.
7. Remove the cap.

For the search of the leaks we recommend the use of electronic device. We dissuade the use
of water and soap or other liquids

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Analytical Tuning
Instrument has been factory – tuned and tested using the following sample mixtures:

Test Mix 1
Component Concentration %
H2 1.10
Methane Matrix

Test Mix 2
Component Concentration %
Methane 1.10
Ethane 1.10
Ethylene 1.10
Propane 1.10
Propylene 1.10
n - Butane 1.10
1 - Butene 1.10
n - Pentane 1.10
1,3 - Butadiene 1.10
Pentene 1.10
Cis 2 - Pentene 1.10
n-Hexane 1.10
Helium Matrix

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Analytical Separation
A schematic of the separation performed by the analyzer are the following:

Hydrogen channel
Step 1
The hydrogen channel comprises a gas sample valve injecting directly onto a
combination of molecular sieve and porous polymer column in series. The sample is
injected onto the columns where the separation of the hydrogen is made from the
remaining components.

Step 1

Step 2
Once Hydrogen is eluted, the columns are placed in reverse flow and the remaining
components are send to vent.

Step 2

Hydrocarbons channel
Step 1
This channel comprises a gas sampling valve injecting into a split/splitless injector.
The operator can therefore choose the ideal split ratio for the sample to be analyzed
or to use the recommended split ratio. The sample is then passed onto a capillary
column. The detector used on this channel is a Flame Ionization Detector (FID).

Step 1

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Analytical Parameters
Parameter Value
Injector
Left SSL Temperature 200° C
DPFC Mode Constant Flow
Carrier Gas Flow 2.5 ml/min
Mode Split
Split flow 120 ml/min
GC1 (A) Pressure 100 kPa
GC2 (B) Pressure 40 kPa
Detector
Left FID Base temperature 200°C
Air Flow 350 ml/min
Hydrogen Flow 35 ml/min
Make up Flow 30 ml/min
Right TCD Block Temperature 200°C
Transfer Temperature 190°C
Filament Voltage 10 V
Max Filament Temperature 400°C
Make-Up Flow 10 ml/min
Reference Flow 30 ml/min
Oven
Initial Temperature 80°C
Initial Time 1 min
Rate 10°C/min
Final Temperature 160°C
Final Time 10 min
Valve Oven Temperature 50°C
Run Table Hydrogen Channel
Time Valve# Position
00.01 Valve# 2 Sampling Inject for 0.70
Run Table Hydrocarbons Channel
Time Valve# Position
00.01 Valve# 3 Sampling Inject for 0.30

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Analytical Result
Typical chromatograms produced in previous condition are reported in figure 1-2

Figure 1-2 Typical chromatogram of Test Mix1 on Hydrogen Channel

Red Chromatogram: Analysis without backflush
Blue chromatogram: Analysis with backflush

Test Mix 1
Retention Time Component Name
0.540 H2
1.653 Methane

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 Typical chromatograms produced in previous condition are reported in figure 1-3

Figure 1-3 Typical chromatogram of Test Mix2 on Hydrocarbons channel

Retention Time Component Name

4.750 Methane
4.930 Ethane
5.103 Ethylene
5.442 Propane
6.175 Propylene
6.775 n - Butane
8.083 1 - Butene
9.160 n - Pentane
9.475 1,3 - Butadiene
10.855 Pentene
11.130 Cis 2 - Pentene
12.610 n - Hexane

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Troubleshooting
The following solutions can fix the most common problems generated during the
operation of the analyzer.

Loss of chromatographic resolution

A loss of resolution is generally caused by dirty columns (water and other
components in the sample absorbed by the column). To short out this
problem, proceed with the conditioning of the column as described in the
related section.

Increase of the Height of Interfering Peaks and Switching Disturbs

After some time the instrument is in stand by mode, some air may diffuse through the valves,
contaminating the columns and compromising the analytical result. To overcome this
problem it is sufficient to run 3 or 4 blank analyses (without sampling) with a different run
time program which speeds up significantly the blank analysis.

Consumables
Part Number Description
PKBA00000006000 Column: 1 m, 1/8” Haysep Q, 60-80 mesh
PKBA00000010000 Column: 1 m, 1/8” Molecular Sieve 13X, 60-80 mesh
RT-19701 Column: 50 m, 0.53 ID Alumina, 6 µm film thickness
27207026 1 ml sampling loop
27207029 0.25 ml sampling loop

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