Manual For 7890-0261 - Rev D TOGA
Manual For 7890-0261 - Rev D TOGA
INTRODUCTION ..................................................................................................................................5
CALIBRATION...................................................................................................................................20
INTRODUCTION
The Agilent 7890 GC analyzer for Transformer Oil Dissolved Gases is designed to measure the
gases in the head space of transformer oil, including hydrogen, oxygen, nitrogen, ethylene, ethane,
acetylene, propane, propylene, 1-butene, carbon monoxide, and carbon dioxide. The carrier gas
recommended is Argon.
A procedure for analyzing the gas using a Head Space Sampler is described in ASTM Method
D3612, section C. It is strongly recommended that a copy of this ASTM method is on hand. The
quantitative standards necessary for instrument calibration can be purchased from many gas
suppliers. A gas mixture containing the gases of interest at a level of about 50 ppm in a balance of
Argon is suggested.
In this system for normal use, the sample is injected from the head space sampler onto two PLOT
columns in series. A special “inlet” is supplied that allows the transfer line of the G1888A or 7697A
Head Space Sampler to be connected to the GC.
To make calibration easier, a gas sampling valve is built into the GC so that an accurate calibration
gas can be injected without the need of filling sample vials up with calibration gas.
The analyzer uses a 30 meter x 0.53mm x 50um Molecular Sieve 5A column and a 30 meter x
0.53mm x 40.0um HP-PLOT-Q column.
Please note that this column combination is not exactly the same as the ASTM method. Work
at Agilent has shown that the Carbon Plot type columns do not reliably allow the
measurement of low levels of oxygen. For this reason we have moved over to the HP-PLOT-Q
column which will separate all of the C2 hydrocarbons and allow the measurement of low
levels of oxygen.
At the start of the run, the valve #1 in the GC is in the OFF position. The Head Space Sampler will
take the allotted vial and deliver it to the sampler oven. Here it will equilibrate and be shaken for the
time mentioned in the ASTM method. The sampler will then inject the head space into the GC and
start the run. If a calibration gas is being analyzed, then the injection will be done by valve 2.
The hydrogen, oxygen, nitrogen, methane and carbon monoxide pass through the HP-PLOT-Q
column into the Molecular Sieve Column. The valve # 1 is turned to the ON position, trapping these
compounds on the Molecular Sieve column. Carbon Dioxide now elutes from the HP-PLOT-Q
column where it is converted to methane by the nickel catalyst and detected in the FID. The C2
gases, Acetylene, Ethylene and Ethane now elute from the HP-PLOT-Q column.
There is about a 4 minute time gap between the elution of the last C2 peak, ethane, and the first C3
peak, propylene. During this time the valve # 1 is switched back to the OFF position, allowing the
gases trapped on the Molecular Sieve column to elute. The first three peaks, hydrogen, oxygen and
nitrogen are detected on the TCD. The other two peaks, methane and carbon monoxide are
After the carbon monoxide has eluted, the valve is switched back to the ON position, enabling the
C3 and C4 hydrocarbons to elute from the HP-PLOT-Q column.
Typical checkout sample chromatograms are included on the CD provided. Typical retention times
and elution order are shown in the chromatograms below for the FID and TCD channels.
A calibration gas mixture should be at the 50 ppm level and contain at least the following gases:
Hydrogen, nitrogen, methane, carbon monoxide, carbon dioxide, acetylene, ethylene, ethane,
propane and if needed propylene and any C4 hydrocarbons. The balance gas should be Argon.
The Gas Chromatograph should have Argon carrier gas connected to channel 1 of the Pneumatics
Control Module, the vial pressure inlet of the head space sampler and to the Thermal Conductivity
Detector. Hydrogen and Air should be connected to the Flame Ionization Detector. Air should also
be connected to the valve actuators; this is the ¼ inch plastic tubing.
The Head Space Sampler should be placed on the right side of the GC. Connect the line coming out
of the primary PCM channel from the GC marked ‘Carrier’ to the Carrier inlet of the Head Space
Sampler.
Connect the heated transfer line of the Head Space Sampler to the special inlet fitting on the GC.
An Ultimetal treated metal tubing, part number CP6530, is supplied to be used for the transfer line.
First connect one end of the line into the valve of the Head Space Sampler, see pages 36 to 38 of
the Head Space Installation manual. When this has been installed and the covers replaced, you will
need to prepare the other end of the tubing.
Slide the M5 adapter, part number G2319-20210, onto the metal tubing and slide it up to the black
plastic end cap of the heated line until it is a close fit to the cap. Slide a vespel ferrule, part number
G3445 Option 571 and G3440 SP1 7890-0261 Printed Copies
Rev. D are Uncontrolled
Agilent Technologies, Inc. Page 9 of 30 Date Printed: 27 November 2013
5062-3538 onto the tubing and slide it up the tubing until it is in contact with the M5 adapter. Cut the
tubing with a ceramic column cutter about 5 mm from the end of the ferrule, as shown in the picture
above.
With a finger holding the ferrule in place, insert the transfer line into the GC ‘inlet’ and tighten the M5
adapter using a ¼ inch wrench. Do not over tighten. The safest way is to set a flow of 15ml/min of
carrier gas through the columns using the PCM. Monitor the pressure, and as soon as it starts to
rapidly increase, tighten an extra ½ turn. Clamp the heated transfer assembly to the GC using the
supplied clamp with the Head Space Sampler.
Connect the Remote Start Stop cable, P/N G1290-60575 supplied with the Head Space Sampler,
from the Sampler to the Remote connector on the rear of the GC.
The calibration mixture should be at the 50 ppm level and contain at least the following gases:
Hydrogen, nitrogen, methane, carbon monoxide, carbon dioxide, acetylene, ethylene, ethane,
propane and if needed propylene and any C4 hydrocarbons. The balance gas should be Argon.
Column #1
Agilent TOGA column set30 m Plot Q + 25 m Molesieve 5
250 °C: Packed
In: PCM C-1 ArMe
Out: Front Detector FID
Flow Program On
6.8948E+05 mL/min for 0 min
Run Time 13.917 min
=====================================================================
Agilent 7697A
=====================================================================
Headspace Device: Agilent 7697A()
Address: 130.30.233.70
Serial Number: CN11140015
Firmware Revision: A.01.02
Instrument Settings
Vial Pressurization Gas: Helium
Loop Size (mL): 1
Pressure Units: psi
Keyboard Lock: ON
System Configuration
Instrument Controlling Carrier GC Instrument
Resource Conservation
Vial Standby Flow: OFF
Temperature Settings:
Oven Temperature: 70
Loop Temperature: 150
Transfer Line Temperature: 150
Timing Settings:
Vial Equilibration (min): 0.10
Injection Duration (min): 0.50
GC Cycle Time (min): 15.00
Vial and Loop Settings:
Vial Size: 20 mL
Vial Shaking: Level 5, 71 shakes/min with acceleration of
260 cm/s²
Fill Mode: Flow to Pressure
Fill Flow: 150
Fill Pressure (psi): 20
Fill Time: 0
Loop Fill Mode: Custom
Loop Ramp Rate: 199 psi/min
Loop Final Pressure (psi): 0
Loop Equilibration Time (min): 0.5
Carrier Control Mode: GC controls Carrier
Advanced Settings:
G3445 Option 571 and G3440 SP1 7890-0261 Printed Copies
Rev. D are Uncontrolled
Agilent Technologies, Inc. Page 12 of 30 Date Printed: 27 November 2013
Extraction Mode: Single Extraction
Vent After Extraction: ON
Post Injection Purge: 30 mL/min for 5 min
Acceptable Leak Check: OFF mL/min
Sequence Actions:
Vial Missing: Skip
Wrong Vial Size: Continue
Leak Detected: Continue
System Not Ready: Continue
3. Valve 1 is OFF
4. Carrier gas and Vial Pressurization channels (from PCM or Aux EPC) are ON
Oven 70°C
Loop 150°C
Transfer Line 150°C
As supplied from the factory, the columns will have been conditioned. If the GC has been in storage
for some time, the columns may need to be re-conditioned.
3. Set Valve 1 to ON
4. Set the Oven temp to 250°C. Allow to run for two hours or until the base line is stable.
6. Allow to run for another two hours or until the baseline is stable.
4. Monitor the pressure for the front inlet. When it is stable, make a note of the value.
6. Adjust the needle valve to give the same pressure as noted above.
If ChemStation is being used as the data system, set the ‘Injection source’ to ‘Manual’.
Make sure that the only entries in the run table are as follows.
1. Set the pressure of PCM C Aux pressure to 5 psi or whatever pressure you will use for the
Head Space Sampler loop pressure.
2. Connect a flow meter to the PCM C Aux pressure Swagelok fitting at the rear of the GC.
When viewed from the rear of the GC, this will be the fitting on the left of the PCM module.
3. With the calibration connected to sample line inlet, increase the pressure at the calibration
gas bottle until the indicated flow is about 20ml/min.
4. Allow to flow for about 30 seconds.
5. Turn the calibration gas OFF at the gas bottle.
6. Press ‘Start’ run on the GC.
7. Turn PCM C Aux pressure to OFF.
Fill the sample loop and start the run. The chromatogram on the FID channel should be similar to
that shown below.
Note the time for the third peak, in this case 1.680
Subtract the time for the second peak from this time. (1.680 – 1.552 = 0.128)
Add this result to the retention time for the second peak (1.552+ 0.064 = 1.616). We will call this
Time A.
Valve 1 ON = Time A
Note Time B. This is the time when the sixth peak has finished plus 0.1 minutes. Enter into the Time
table
Note Time C. This is the start time of the seventh peak minus 0.2 minutes. Enter into the Time table
Valve 1 ON = Time C
To finish off, note the total run time for the GC. Subtract 0.05 minutes from this time and call it Time
D. Enter the following into the Time table.
The system is now ready to use. However, first save the method on the ChemStation.
Note: If it is not possible to get the carbon monoxide to elute from the Molecular Sieve
column before switching for the elution of the propylene peak, it may be necessary to
shorten the Molecular Sieve column. This should be done by removing one loop at a time
from the Molecular Sieve column until the carbon monoxide peak elutes within the time
frame.
Before proceeding with Head Space analysis, remove all entries for Valve 2 from the run
table.
Ensure that for the Signal Description, there is a line for the FID and the TCD. If one of these is
missing, go to the ‘Available Signals’ box, select the missing detector, and click the ‘Add to Method’
button.
The report needs to be set up for ESTD and sorted by retention time. To do this, make sure that you
are in the ‘Data Analysis’ view, click on the ‘Report’ and ‘Specify Report’ menus, and the following
will appear.
We will assume that the GC has been calibrated in ppm (v/v). This will give us the concentrations of
the gases in the GAS phase. The formula to get the concentration of the gases in the liquid phase is
CL=CG(K+VG/VL)
Where
CG = concentration of the gas in the gas phase.
K = partition coefficient for the gas
VG = Volume of the gas phase in the vial
VL = Volume of the liquid phase in the vial
The Chemstation allows you to set up a multiplier factor for each compound in the calibration table.
To do this, proceed as follows.
You will first need to have a calibration table prepared for this analysis. You will also need to have
the Multiplier column visible as shown below
Click on Calibration/Calibration Table Options/Edit Options. If you do not see the ‘Edit Options’
choice, you will need to go to ‘View’ and then click on ‘Full Menu’.
Select ‘Multiplier’ in the list of ‘Columns not shown’ and then click on the -> button to move it over
into the list of ‘Columns shown’, and click ‘OK’. The Multiplier column will now be part of your
calibration table. You will now need to calculate the multiplier factor for each compound. This is the
partition coefficient plus the ratio of the gas phase to liquid phase. Using the numbers from the
ASTM method we would calculate the factor for hydrogen as
This is assuming that we have found that the TOTAL volume the vial is 20.61mls and that we have
added 15.0 ml of oil. Similarly for ethane gas we would get a factor of
The Chemstation will now give the amounts of the gases in the oil. If you multiply the total amount
given in the Chemstation report by 10-4, you will get the total percentage of gas in the oil (See ASTM
method).
The columns are supplied with particle traps. These traps are installed on the EXIT of each column
to prevent small column particles that may become dislodged, from entering the valve. If the
particles were to enter the valve they could score the sealing surfaces which would result in air
leaking into the system.
The columns should be installed such that the HP-PLOT-Q is the rear column and the Molecular
Sieve column is at the front. When they are installed, the EXIT of the HP-PLOT-Q column will be on
the right side of the oven. The particle trap for the HP-PLOT-Q column will therefore be connected to
the rear bulkhead fitting on the right side of the oven.
The EXIT of the Molecular Sieve column will also be on the right side of the oven. The particle trap
for the Molecular Sieve column should be connected to the front bulkhead fitting on the right side of
the oven.
Cut the standard 2.5m particle trap, part number 5181-3352, in half.
For good sealing it is important that the cut is 90 degrees to the trap and the cut is clean. A suitable
cutting tool is supplied by Agilent Technologies and may be ordered using the part number 5183-
4620.
Remove the old trap from the column by cutting off the old trap and connector using a suitable cutter
as mentioned above.
Install the end of the column into a microfluidics type column connector part number G3182-61581
using the swaging nut contained in the kit and the appropriate ferrule for the megabore column
(order P/N 5188-5363 10 pk).
Reconnect the trap to the bulkhead fitting, using a new Siltite ferrule if needed.
Microfluidics type
connector
Ferrule 0100-1512
The Gas Chromatograph should have Argon carrier gas connected to both channels of the
Pneumatics Control Module and to the Thermal Conductivity Detector. Hydrogen and Air should be
connected to the Flame Ionization Detector. Air should also be connected to the valve actuator; this
is the ¼ inch plastic tubing.
The Head Space Sampler should be placed on the left side of the GC. Connect the line coming out
of the primary PCM channel from the left side of the GC marked ‘Carrier’ to the Carrier inlet of the
Head Space Sampler. The PCM also have a secondary channel pressure control, and such channel
will have a connector which should be connected to the Head Space Vial Pressurization inlet. Set
the G1888A for EPC control. See the Users Manual Page 32.
Connect the heated transfer line of the Head Space Sampler to the special inlet fitting on the GC.
You will need a 7mm wrench to tighten this up. This wrench is supplied with the Head Space
Sampler.
Connect the Remote Start Stop cable, P/N G1290-60575 supplied with the Head Space Sampler,
from the Sampler to the Remote connector on the rear of the GC.
A gas sample will be needed to check out the system. A suitable sample is part number G3440-
85007 from Agilent Technologies.
A suitable calibration mixture should be at the 50 ppm level and contain at least the following gases:
Hydrogen, nitrogen, methane, carbon monoxide, carbon dioxide, acetylene, ethylene, ethane,
propane and if needed propylene and any C4 hydrocarbons. The balance gas should be Argon.
Please see Appendix A for description of a method to fill the sample loop with a calibration gas
without the need for filling a vial with gas.
Set the following method into the GC. The method may also be loaded from the CD-ROM supplied
with your instrument.
=====================================================================
Agilent 7890 GC
=====================================================================
Oven
Oven On
Equilibration Time 0.5 min
Oven Program
40 degrees C for 6 min
then 24 °C/min to 230 degrees C for 0 min
Column #1
Agilent toga: 300 °C: Packed
plot Q + plot MOLESIEVE: 173.61175
In: PCM C-1 ArMe
Out: Front Detector
Valve 1
Other Off
PCM C-1 On
Carrier Gas ArMe
Flow Program
15 mL/min for 14 min
PCM C-2 On
Carrier Gas ArMe
Channel B Control Mode Forward Pressure
Pressure Program
10 psi for 0 min
Signals
Front Signal Save On
Back Signal Save On
Test Plot Save Off
Test Plot Save Off
1. Column is defined as a packed column and assigned to the PCM C-1 channel. This ensures
that the PCM module can be in a constant flow mode measured in the PCM and not as a result of a
capillary column calculation. To configure the PCM channels, please refer to the 7890 User Manual
and ChemStation documentation.
2. Valve 1 is ON
3. Carrier gas and Vial Pressurization channels (from PCM or Aux EPC) are ON
Oven 70°C
Loop 150°C
Transfer Line 150°C
First Vial 1
Last Vial 1
Shake High
Note: If the calibration gas is being supplied from the vent line (See Appendix A), then set the ‘Vial
Equilibration time’ to 1.0 minute.
As supplied from the factory, the columns will have been conditioned. If the GC has been in storage
for some time, the columns may need to be re-conditioned.
The Headspace sampler is supplied with a 1 ml sample loop installed as standard. This analyzer
has been checked out with this sample loop size. This has been found to be adequate and gives
improved peak shapes. The set points given above assume that a 1ml sample loop is being used.
A 3 ml sample loop is supplied as a spare loop with the headspace sampler. In the event that you
feel that this is needed, you should be aware that the system will need to be operated under different
conditions. The set points above run the GC in a constant flow mode. If you run with the 3ml loop
then you should run the GC in constant pressure or ramped pressure mode. This will ensure that the
loop fills up quicker with carrier gas when the sampling valve is switched, which will improve the
peak shape.