Installation and Operation

of Gas Analyzer for

Transformer Oil with Head
Space Sampler

Specials and Solutions Group

For use with G3440 SP1 7890-0552
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 7890 TRANSFORMER OIL GAS ANALYSIS
Using a Head Space Sampler

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, sample is injected from the head space sampler onto three PLOT columns in series.
A special inlet is supplied that allows the transfer line of the G7697A or G1888A Head Space
Sampler to be connected to the GC.

The system allows the customer to backflush compounds that are not of interest and thus speed up
the analysis and to also bypass the nickel catalyst when needed.

A gas sampling valve has been added to the valve configuration to make it easier to introduce a
calibration gas. This is used in conjunction with electronic back pressure control so that the
calibration gas can be injected under the same conditions as used by the injection valve inside the
Head Space Sampler.

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.

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THEORY OF OPERATION

A system diagram is shown below. It is recommended to follow the explanations of this section
referencing to this graphic. For other possible configurations, please see Appendix 3.

FLOW
Valve System
INJECTION VALVE COMPARTMENT
Date :
Order No :
S/N :

Item :
DETECTOR
OVEN LEFT SIDE
SOURCE PORT BLOCK 2 BLOCK 1

= #872 4/701 1/700

4
4 3
Back Aux 5
3
5
6
Ch 2 6 1
2 Side
2
LOOP
PCM C 1

Ch 1
IN
Back Inl
Argon Back SAMPLE
CP6533 2m x 0.010' (0.25mm) Back
CAT
FID H2 In
(307) TCD
160-2325-1 (220)
Front Inl Front Cut to 0.45 m x 0.320mm
CP6530 Front

HSS Col 1 Col 3

FID
Interface
(210)
4 4
Front Aux 3
Carrier 5
3 5
Ch 2 6
HSS 6 2 2
PCM A Vial
1 1

Ch 1 pressurization

Argon Col 2
3/700/3x872 2/702/3x872
Options SP1 options Remarks

210,220,307,2x309,2x700,701,702,754,7x872 7890-0552 PCM C Channel 2 in back

pressure mode

Column 1 CP-PoraBOND Q 10m x 0.53mm x 10m

Column 2 HP-PLOT Q, 30m x 0.53mm x 40um
Column 3 HP PLOT MolSieve 30m x 0.53mm x 50um

At the start of the run, the valves in the GC are 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.

The hydrogen, oxygen, nitrogen, methane and carbon monoxide pass through the PoraBOND Q
pre-column and HP-PLOT-Q column into the Molecular Sieve Column. The valve # 2 is turned to the
ON position after trapping these compounds in 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. Then the valve #1 is switched ON, the C2 gases [Acetylene, Ethylene and
Ethane] now elute from the HP-PLOT-Q column and are detected by FID directly. The valve #3 is
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turned ON at appropriate time to backflush possible C4+ hydrocarbons in PoraBOND Q pre-column
so as to shorten analysis time.

There is about a 4 minutes time gap between the elution of the last C2 peak [ethane] and the first C3
peak [propylene]. During this time the valve # 2 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
detected on the FID. For the carbon monoxide, this is accomplished by first converting the carbon
monoxide to methane on the nickel catalyst.

After the carbon monoxide has eluted, the valve #2 is switched back to the ON position, enabling the
C3 hydrocarbons to elute from the HP-PLOT-Q column.

Installation

Understand the application requirements for carrier and support gases before connecting them. The
Gas Chromatograph should have Argon carrier gas connected to both primary channels of the EPC
A and C and to the Thermal Conductivity Detector and to the vial pressurization inlet on the HSS.
Hydrogen and Air should be connected to the Flame Ionization Detector. Air should also be
connected to the valve actuators; this is the inch plastic tubing at the rear of the instrument.
Supply them with clean air which is oil, water and particulates free at about 40 psi constant. Power
up the GC.
Start by setting the correct communication parameters in the GC found by pressing the keys
[OPTIONS] and then scrolling to "Communications" and pressing [ENTER]. Once done, reboot the
GC.
If this is the only factory tested method, then the checkout method set up for the instrument will be
stored in Method # 9 GC memory position. Load the GC method pressing [LOAD] [METHOD] [9]
in the GC keyboard or manually enter the parameters found in the method text file found in the
analyzer CD using the GC keyboard. Allow the system to stabilize.
If an Agilent Open Lab ChemStation rev. C.01.05 (or higher) is installed in the work station (PC)
start the "Open Lab Control Panel" by clicking in the corresponding icon. Once open, left click the
"Configure Instrument" icon (round purple button with tools) and wait for the next screen opens.
Once opened, check that the selection for "Method Load on Startup" condition is set to "Always ask
user to choose an option". Then proceed to move one "7890 GC" icon from the "Configurable
Modules" selection in the left field of the screen to the "Selected Modules" field visible at the right of
the screen. Double click on the 7890 GC icon just moved in the previous operation and type the
required information in "Connect Info". Most important is the IP address and other communication
parameters previously set in the GC. Once this is done, immediately click the "Get GC
Configuration" button and allow a few seconds for the communication to establish. If a positive
communication success message displays, then the Open Lab ChemStation has received and
stored the specific configuration of that GC (Inlets, detectors, valves, etc.). Review the
"Configuration" tab and verify that matches the actual instrument. Exit this screen by pressing "OK".
Once back in the "Configure Instrument" screen, exit from there too by pressing "OK" button again.
Now start the instrument just configured pressing the round purple icon named "Launch". After a few
seconds, a screen labeled "Choose Method Load Option" will come up if this is the first time the
control software is used. In this case choose the option "New Method from Instrument" which will
take you to the ChemStation control screen under a default method (def_gc.m) which has the same
GC control parameters loaded as the method shipped in the memory of the GC (provided that it was
loaded as instructed before), but won't contain any data analysis parameters like the calibration table
for the checkout standard. This is when the factory tested method needs to be loaded from the
Specials CD (found in the Specials ship kit) into the computer and from it to the ChemStation.
For this analyzer the method to be loaded is 7890-0552.M

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Allow the GC to equilibrate for a length of time adequate for the application (detectors baseline,
column purge time, etc.).

=====================================================================
Agilent 7890B
=====================================================================

GC
Oven
Equilibration Time 0.5 min
Max Temperature 250 C
Slow Fan Disabled
Oven Program On
Oven Program 40 C for 5.5 min
Oven then 20 C/min to 130 C for 0
min
Run Time 10 min
Cryo Off

Thermal Aux 1 (Nickel Catalyst)

Heater On 375 C

Column

Column #1

Porabond Q + MSPlot 5A + Plot Q

0 C325 C (250 C): 70 m x 530 m x 50 m
Column lock Unlocked
In PCM C-1 ArMe
Out Front Detector FID
(Initial) 40 C
Pressure 33.901 psi
Flow 15 mL/min
Average Velocity 76.637 cm/sec
Holdup Time 1.5223 min
Flow Program On
Flow Program 15 mL/min for 0 min
Run Time 10 min

Column #2

MSPlot 5A + Plot Q
0 C250 C (325 C): 60 m x 530 m x 50 m
Column lock Unlocked
In PCM A-1 ArMe
Out Back Detector TCD
(Initial) 40 C
Pressure 30.638 psi
Flow 15 mL/min
Average Velocity 81.458 cm/sec
Holdup Time 1.2276 min
Flow Program On
Flow Program 15 mL/min for 0 min
Run Time 10 min

Front Detector FID

Heater On 250 C
H2 Flow On 60 mL/min
Air Flow On 500 mL/min
Makeup Flow On 25 mL/min
Carrier Gas Flow Correction Does not affect Makeup or Fuel Flow
Flame On
Electrometer On

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Back Detector TCD
Heater On 250 C
Reference Flow On 20 mL/min
Makeup Flow On 2 mL/min
Negative Polarity On
Filament On
Valve 1
Other Off
Valve 2
Other Off
Valve 3
Other Off
Valve 4
Other Off
PCM
PCM A-1 ArMe
PCM A-1 ArMe Supplies Column 2

PCM A-2 N2
Pressure Program Off
Pressure Program 5 psi for 0 min
Run Time 10 min

PCM
PCM C-1 ArMe
PCM C-1 ArMe Supplies Column 1

PCM C-2 ArMe

***Excluded from Affecting GC's
Readiness State***
Pressure Program On
Pressure Program 5 psi for 0 min
Run Time 10 min

Valve Box
Heater On 70 C

Signals
Signal #1: Front Signal
Description Front Signal
Details
Save On
Data Rate 5 Hz

Signal #2: Back Signal

Description Back Signal
Details
Save On
Data Rate 5 Hz
Signal Events#2
Signal Events#2 Time 4.8 min
Signal Events#2 Event Resume Signal

Signal Events#2 Time 6.8 min

Signal Events#2 Event Freeze Signal

Signal Events#2 Time 0.02 min

Signal Events#2 Event Freeze Signal

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Run Time Events
Run Time Events
Run Time Events Time 0.05 min
Run Time Events Event Valve
Run Time Events Position Valve 4
Run Time Events Setpoint On
Run Time Events Time 1 min
Run Time Events Event Valve
Run Time Events Position Valve 4
Run Time Events Setpoint Off

Run Time Events Time 2.55 min

Run Time Events Event Valve
Run Time Events Position Valve 2
Run Time Events Setpoint On

Run Time Events Time 3.2 min

Run Time Events Event Valve
Run Time Events Position Valve 1
Run Time Events Setpoint On

Run Time Events Time 4 min

Run Time Events Event Valve
Run Time Events Position Valve 3
Run Time Events Setpoint On

Run Time Events Time 4.6 min

Run Time Events Event Valve
Run Time Events Position Valve 2
Run Time Events Setpoint Off

Run Time Events Time 7.4 min

Run Time Events Event Valve
Run Time Events Position Valve 1
Run Time Events Setpoint Off

Run Time Events Time 8.6 min

Run Time Events Event Valve
Run Time Events Position Valve 2
Run Time Events Setpoint On

Run Time Events Time 8.7 min

Run Time Events Event Valve
Run Time Events Position Valve 1
Run Time Events Setpoint On

Run Time Events Time 9.5 min

Run Time Events Event Valve
Run Time Events Position Valve 2
Run Time Events Setpoint Off

Run Time Events Time 9.5 min

Run Time Events Event Valve
Run Time Events Position Valve 3
Run Time Events Setpoint Off

Run Time Events Time 9.95 min

Run Time Events Event Valve
Run Time Events Position Valve 1
Run Time Events Setpoint Off

Note: The events marked in RED are only required for calibration injections using the gas sampling
valve (Valve # 4) included in the valve configuration. Remove them from the method time events
table when using the Head Space for sample injection/analysis.

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Connect G7697A HSS
The G7697A Head Space Sampler should be placed on the right side of the GC. Connect the line
coming out of the EPC from the rear side of the GC marked "To HSS Carrier" to the carrier inlet of
the Head Space Sampler, and another line straight from the wall gas source into the supply marked
"HSS Vial Pressure" in the Head Space rear panel.

The transfer line is Ultimetal tubing (P/N CP6530) supplied with analyzer. Connect the transfer line
to Head Space Sampler valve as described in the HSS manual [7697A Headspace Sampler
Installation and First Startup] - Chapter 1 - section [Connect the Transfer Line to the GC].

Trim the metal capillary

tubing to ~5 mm past the
ferrule tip

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
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 pictures
above.

With a finger holding the ferrule in place, insert the transfer line into the GC inlet and tighten the M5
adapter using a 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 turn. Clamp the heated transfer assembly to the GC using the
supplied clamp with the Head Space Sampler as shown in the previous picture

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.

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Connect G1888A HSS
The G1888A Head Space Sampler should be placed on the left side of the GC. Connect the line
coming out of the EPC from the left side of the GC marked "To HSS Carrier" to the Carrier inlet of
the Head Space Sampler, and another line straight from the wall gas source into the supply marked
"HSS Vial Pressure" in the Head Space rear panel. Set the G1888A for Manual control on the
Vial Pressurization channel and for EPC control on the Carrier channel. 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.

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Setup HSS conditions

Set the following conditions on the Head Space Sampler.

Oven 70C
Loop 150C
Transfer Line 150C

GC Cycle Time 13 minute

Vial Equilibration time 30.0 minute
Pressurization time 0.25 minute
Loop fill time 0.25 minute
Loop equilibration time 0.25 minute
Inject time 0.90 minute

First Vial 1
Last Vial 1
Shake High

Note: If the calibration gas is being supplied from the vent line, then set the Vial
Equilibration time to 1.0 minute and Shake to OFF. For G7697A, below parameters are
recommended.

Vial Fill Mode: To Pressure

Vial Fill Pressure: 5 psig
Vial Pressure Hold Time: 1 minute
Vial Standby Flow: 30 ml/min

A gas sample will be needed to check out the system. A suitable sample is supplied by Agilent
Technologies under the part number G3440-85007.

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. The balance gas should be Argon.

There are several ways to get the calibration gas from the Head Space Sampler into the GC. The
first is to use the procedure outlined in the ASTM D3612 method. This involves filling Head Space
vials with the calibration gas.

A second way (preferred for simplicity) involves the use of the gas sampling valve in the GC that is
supplied with the same size gas sample loop (1ml) as that used in the Head Space Sampler. The
valve has a gas sample IN line (2.0 m X 0.01 in ID) and a gas sample OUT line. The OUT line is
connected to the second channel of PCM (Pneumatics Control Module) C which must be set up in
Back Pressure mode. This will then enable the calibration gas to be injected at the same pressure
as that used in the Head Space Sampler (see the Head Space method parameters).

For customers using the G1888A Head Space Sampler

A third method has been used successfully in the factory for checking out the system with the
G1888A Head Space Sampler. However, you should first review the safety aspects. The Head
Space Sampler has a gas sampling valve built into it. The sample loop is normally filled by
pressurizing the vial, and then allowing the vial to depressurize to a vent via the sample loop (See

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your head space manual for the details). A method developed in the factory supplies the calibration
gas to the vent at the rear of the sampler, and installing a vial with no cap on it. The sample loop will
be filled in the opposite direction, that is, the gas will flow from the vent into the vial. However it
must be realized that the calibration gas will escape into the head space oven. At
concentrations of 50 ppm in Argon, and the relative short time that the gas flows and the fact that the
oven is open to the atmosphere, no large build up gases should occur. If you have any doubts in
using this technique, then use the standard ASTM method of using vials filled with the
calibration gas.

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Checkout procedure

Load the 7890-0552.M method into the online ChemStation and allow the GC instrument to
get ready. Setup the Head Space Sampler parameters according to ASTM D3612 or customer
in-house method. Inject a suitable calibration gas into the GC. Typical retention times and
elution order are shown in the chromatograms below for the FID and TCD channels.
FID1 A, Front Signal (HSSX 2011-08-10 11-52-29\001F0101.D)
pA

FID Channel

Carbon Monoxide
450

400

Propylene
350

300

Propane
Acetylene

250
Ethylene
Carbon Dioxide

200
Ethane

150

Methane
100

50

0
1 2 3 4 5 6 7 8 9 min

TCD2B, Back Signal (HSSX2011-08-1011-52-29\001F0101.D)

25 V
TCD Channel
Hydrogen

-32

-34

-36

-38
Nitrogen
Oxygen

-40

1 2 3 4 5 6 7 8 9 min

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Procedure for a New Setup
This procedure will have to be carried out if new columns are installed. It is recommended to
follow this process in the same order given in this manual. As supplied from the factory, the
pre-installed columns have been conditioned. If the GC has been in storage for some time, the
columns may need to be re-conditioned.

Condition columns
1. Set the column 1 and 2 flow to 15 ml/min.

2. Set Valve 1, 2 and 3 to ON.

3. Set the Oven temp to 250C. Allow to run for two hours or until the base line is stable.

4. Set Valve 2 to OFF

5. Allow to run for another two hours or until the baseline is stable.

6. Set Valve 1, 2 and 3 to OFF.

7. Cool the oven to 40C. Check the column connections integrity.

Sample loop size

The Headspace sampler is supplied with a 1ml 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.

If the sample loop is changed, 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 larger
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.

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Set up needle valve
1. Check that the oven is at 40C.

2. Set column 1 and 2 flow to 15ml/min.

3. Turn OFF TCD and FID gases, and connect flow meter to FID vent.

4. Set Valve 1, 2 and 3 to OFF.

5. Monitor the pressure of PCM C-1. When it is stable, note the pressure value as P1, flow meter
reading as F1.

6. Set Valve 2 to ON.

7. Adjust the needle valve that is attached to valve 2 and marked as Restrictor # 1 to give the
same pressure and flow as noted above (P1, F1).

8. Set Valve 3 to ON, and connect flow meter to Valve 3 vent.

9. Adjust the needle valve that is attached to valve 3 and marked as Restrictor # 2 to give the
same pressure and flow as noted above.

10. Turn ON TCD and FID gases.

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Set up Valve Timing
Clear the run table. Check the initial GC conditions as below,

Valve 1 is OFF
Valve 2 is ON
Valve 3 is OFF
Oven Temperature Program: 40oC (5.5min) 20oC/min 130oC (0min)
With the calibration gas in a vial or calibration gas (set to about 5~10 psi) connected to the vent line
as described above, press START on the Head Space sampler. The Head Space Sampler will fill
the loop, inject the sample and start the GC and ChemStation. The run for the FID signal should look
similar to the chromatogram shown below.
FID1 A, Front Signal (FIRSTV125V2ONV3OFF.D)
Norm. FID Channel
Ethylene
Acetylene
Ethane

2500
Carbon dioxide
Methane

2000
Air+CO

1500

Propene
Propane
1000
Time B
Time A
Time C Time D
500

Oven-40C iso-temp
0

2 4 6 8 10 12 min

Enter into the GC Time Table

Valve 3 ON time = 3.0 minutes,

Valve 3 OFF time = 9.9 minutes

Inject the sample and look for the propane peak in the chromatogram. Take note of the propane
peak area. Repeat the injection to ensure area repeatability.
In order to find the ideal backflush time, try increasing Valve 3 ON time in 0.25 min steps and
injecting the same sample, note the propane peak area after each injection. The appropriate time
value for Valve 3 ON event should be the time that got the propane peak area to remain constant
minus 0.20 minutes. This ensures that the C3 compounds (propene and propane) elute completely
from the 10 m PoraBOND Q pre-column into the 30 m HP-PLOT Q analytical columns but C4 is
backflushed to vent and do not ever enter into HP-PLOT Q column.

If from the first time increase for Valve 3 the area of propane doesn't change, then reduce the time
for the valve 3 ON event until the peak starts decreasing its area and then add 0.20 min up to that
time to get the best backflush time. This situation shouldnt be common though.

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Enter into the GC Time table

Valve 2 ON = Time A (the midpoint between the 2nd peak [CH4] and 3rd peak [CO2])
Net effect: Light gases get trapped in the Molecular Sieve column while CO2 and
C2s bypass Molecular Sieve column.
Valve 1 ON = Time B (the end of 3rd peak [CO2] plus 0.20 minutes)
Net effect: C2s and C3s bypass the nickel catalyst
Valve 1 OFF = 9.9 minutes
Net effect: Reset valve #1 for next run
Valve 2 OFF = Time C (the end of 6th peak [C2H6] plus 0.10 minutes)
Net effect: Trapped H2,O2,N2,CH4 and CO can elute from Molecular Sieve column
Valve 2 ON = Time D (the start of 7th peak [C3H6] minus 0.20 minutes)
Net effect: C3s bypass Molecular Sieve column
Valve 2 OFF = 9.9 minutes
Net effect: Reset valve #2 for next run

Press the start run key on the Head Space sampler for next run. Results should be similar to below.

FID Channel

Time E Time F

Enter into the GC Time table

Valve 1 OFF = Time E (after the end of 5th peak [methane])

Net effect: Allow the CO peak to pass through the nickel catalyst for better detection
Valve 1 ON = Time F (before start of 6th peak [propylene] or right after Valve 2 ON event)
Net effect: Isolate the nickel catalyst and prevent the C3 compounds to pass
through it.

Run the checkout or the appropriate calibration standard gas through the system. the result should
look as below.

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 pA
FID Channel

Carbon Monoxide
450

400

Propylene
350

Propane
300

Acetylene
250

Ethylene
Carbon Dioxide
200

Ethane
150

Methane
100

50

0
1 2 3 4 5 6 7 8 9 min

The system is now ready to use. Calibrate the method with the standard gas runs and remove the
time events related to Valve # 4 (the gas sampling valve for standard injection) from the run time
table. Save the method to the ChemStation. If the calibration sample has been supplied to the Head
Space Sampler from the vent line (G188A model only), remove it and let the vent line connection
free.

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.

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Calibration

How to set up signals

The analyzer is using signals from two detectors, but we need both signals to be in the same report
and calibration table. To ensure that this will happen, you will need to do the following.

Go into the Data Analysis view of the ChemStation. Select File and Load Signal menus and in the
resulting window, click on the Signal Details button. The following will appear.

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.

Make sure that under the Quantitative Results section that Calculate is set to ESTD, Based On is
set to Area and Sorted By is set to RT

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Set up calibration table multiplier factor
It is possible to get the results expressed as ppm of gas dissolved in the oil. To get this, you will
need to know the EXACT volume of the vial used and the amount of liquid oil added to the vial. See
the ASTM method on how to measure the volume of the vials. You will also need to know the
partition coefficients of the gases in the oil. The ASTM method also includes the method to
determine these. It also gives a list of partition coefficients of the gases in Voltesso 35 oil at 70C.
We will use these values to show how this can be done.

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

If the multiplier column is not present, proceed as follows.

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.

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Clicking on the Edit Options will result in the following.

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

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 0.074 + 5.61/15.00 = 0.448

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

2.09 + 5.61/15.00 = 2.464.

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).

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Appendix 1. Column Installation

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.

If the particle traps need to be replaced, proceed as follows.

1) Cut the standard 2.5m particle trap, part number 5181-3352, in half.
2) 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.
3) Remove the old trap from the column by cutting off the old trap and connector using a
suitable cutter as mentioned above.
4) Install the end of the column into a microfluidics type column connector part number G3182-
20580 using the swaging nut contained in the kit and the appropriate ferrule for the mega
bore column (order P/N G3188-27503 10 pk).
5) Install the trap into the other end of the connector.
6) Reconnect the trap to the bulkhead fitting, using a new Fleximetal ferrule if needed. See
Appendix 4 with information on how to use the Fleximetal ferrules.

Microfluidics type
connector

HP PLOT-Q Column HP PLOT-Q Column

particle trap

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Appendix 2. G7697A calibration conditions

Injection Source: HSS

=====================================================================
Agilent 7697A
=====================================================================

Headspace Device: Agilent 7697A(HSS)

Vial Pressurization Gas: Ar (or defined as Nitrogen)
Loop Size (mL): 1
Pressure Units: psi
Vial Standby Flow: 30 mL/min

Temperature Settings:
Oven Temperature: 70
Loop Temperature: 150
Transfer Line Temperature: 150
Timing Settings:
Vial Equilibration (min): 1.00
Injection Duration (min): 0.90
GC Cycle Time (min): 13.00

Vial and Loop Settings:

Vial Size: 20 mL
Vial Shaking: OFF
Fill Mode: Pressure
Fill Pressure (psi): 5
Fill Time: 1
Loop Fill Mode: Default

Carrier Control Mode: GC controls Carrier

Advanced Settings:
Extraction Mode: Single Extraction
Vent After Extraction: OFF

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Appendix 3. Other configuration.

For customers that are using the G1888A Head Space Sampler or do not wish to use a gas
sampling valve to inject the calibration gas, the following configuration will be supplied.

= #872 1/700/872

4
3
Back Aux 5
6 2
Side
1 1

AUX 2
3
Back Inl Back
Back
CAT
(307) TCD
FID H2 In Fused silica (220)
Front Inl Front tube
Front

HSS
FID
Interface
(210)
4 4
Front Aux 3 3
Carrier 5 5

6 6
HSS 1
2
1
2

Vial Pressure
0.01 in. Line

3/700/3x872 2/702/3x872

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Appendix 4. UltiMetal Plus Flexible Metal Ferrules
The available UltiMetal Plus Flexible Metal ferrule packages are listed in Table 1 and Figure 1.

Table 1 Available UltiMetal Plus Flexible Metal ferrule packages

Item Part number Ferrule description

1 G3188-27501 0.1 0.25 mm column id, 10/pk
2 G3188-27502 0.32 mm column id, 10/pk
3 G3188-27503 0.45 0.53 mm column id, 10/pk
4 G3188-27504 Plug, 10/pk
5 G3188-27505 0.25 0.32 mm UltiMetal column id, 10/pk
6 G3188-27506 0.53 mm UltiMetal column id, 10/pk

Figure 1 UltiMetal Plus Flexible Metal ferrules

Each UltiMetal Plus Flexible Metal ferrule part number is uniquely designed to prevent inventory mix-
ups, and to help you find the ferrule you need quickly. Color variations between ferrules are a normal
result of the UltiMetal coating.

Tools Required

Two 1/4- inch open- end wrenches

Column cutting tool
Swaging wrench

Preparing the Column Ends

1. Pass the column end through the internal nut, the ferrule, and the swaging wrench (Figure 2).

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 Figure 2 Thread the column through the internal nut, ferrule, and swaging wrench

1. Thread the internal nut into the swaging wrench with the column protruding out of the back of the
wrench (see Figure 3).

Figure 3 Thread the internal nut onto the swaging wrench

2. Begin to swage the ferrule to the column using a 1/4- inch open- ended wrench.

The design of UltiMetal Plus Flexible Metal ferrules reduces the probability of column breakage and
minimizes the damage to the thread of the corresponding fittings.

Unlike other ferrule designs, a reliable leak- free seal is best made by tightening the internal nut to a
recommended number of degrees, not by applying more force. Applying excessive force will not
provide a better seal. Also, compressing the flexible ferrule less minimizes damage to fittings.

To swage the ferrule to the column:

(a). Find your ferrule type in Table 2 and note the range of degrees to tighten the internal nut.

(b). Tighten the internal nut clockwise to the lower end of your ferrules range.

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(c). Check if the ferrule is gripping the column. If yes, stop. If not, continue to tighten the internal nut
in small 5- to 15- degree increments. Check after each increment to see if the ferrule is gripping the
column. Stop as soon as gripping occurs (see Figure 4).

Table 2 Degrees to tighten the internal nut for proper swaging

Ferrule part number Degrees to tighten internal nut

G3188-27501 50 100 degrees
G3188-27502 30 70 degrees
G3188-27503 20 50 degrees
G3188-27504 60 degrees
G3188-27505 40 90 degrees
G3188-27506 20 50 degrees

Figure 4 Tightening the internal nut

3. Using the 1/4- inch open- ended wrench, turn the internal nut an additional 15 to 20 degrees
clockwise to assure the ferrule is properly swaged onto the column (see Figure 5).

Figure 5 Ferrule swaged to column and internal nut.

4. Using the 1/4- inch open- ended wrench, remove the internal nut from the swaging wrench and
column.

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5. Using the column cutter, trim the column at the small end of the ferrule leaving approximately
0.3 mm of the column extending from the ferrule (Figure 6). The minimum size of the column
head extending from the ferrule is 0.1 mm and the maximum is 0.5 mm. It is important to have
0.5 mm or less column head to prevent column conflict in the union.

Figure 6 Properly-trimmed column and ferrule.

Swaging Quality Inspection

Figure 7 shows both an incorrect and correct swaging symmetry.

Figure 7 Incorrect and correct swaging symmetry

If your column and ferrule appear like the incorrect example in Figure 7 above, it is possible that
your swaging wrench is defective or worn out. Try swaging with a new wrench or new nut.

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Summary of swaging the new ferrules.

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