Natural Gas Analyzer

1 Valve

Specials and Solutions Group

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General information

This GC is configured to analyze natural gas according to the ASTM method 1945 and the GPA method 2261. The
analyzer is a one valved system using 1/8 inch packed columns with early back-flush of the C6+ components. A plumbing
diagram is shown below.

.
DATE : 3/18/2002 File
6890 Valve System O/N : ITEM
FLOW INJECTION VALVE COMPARTMENT
BLOCK 2 BLOCK 1 DETECTOR
SOURCE PORT

1/805
Column 2

6 5
7
8 4
OUT
9 3
SAMPLE 10 2
1

IN
Column 1
LOOP
A A
A TCD
PPI
(220)
(102)

6890 Options
102
220
751
805
sa
Fig 1

The columns used in this analyzer are as follows. All are 1/8 inch stainless steel.

Column 1 3 Foot 35% DC200 on PAW 80/100 mesh

Column 2 30 Foot 35% DC200 on PAW 80/100 mesh

The plumbing diagram shows a packed inlet as the flow source for the valves. The pneumatics control module
can also be used as a flow source. Valve 1 is a 10 port valve configured as a gas sampling with sequence reversal and
backflush of the pre-column.

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Analysis Sequence
The diagrams below show the sequence of the analysis

1. Injection and first minute of the run.

DC200 30 Ft DC200 3Ft TCD

C5-C1,CO2,N2 O2 C6+

Note that the sample is injected onto the short DC200 column.

2. Backflush and reverse flow of the short DC200 ensures that C6 and higher compounds come out early in the
chromatogram as one peak.

C5-C1,CO2,N2 O2 C6+

Installation.
Connect all gases to the GC and power up the GC. If a HP ChemStation is being used - bring up the ChemStation and
load the method NatGas1.M (See floppy disc supplied)

Verify the following conditions

=============================================================================
6890 GC METHOD
=============================================================================

OVEN
Initial temp: 130 'C (On) Maximum temp: 225 'C
Initial time: 14.00 min Equilibration time: 0.25 min
Ramps:
# Rate Final temp Final time
1 0.0(Off)
Post temp: 0 'C
Post time: 0.00 min
Run time: 14.00 min

FRONT INLET (UNKNOWN) BACK INLET ()

Flow: 30.0 mL/min (On)
Gas type: Helium

COLUMN 1 COLUMN 2
Packed Column (not installed)
Model Number: Agilent GPA 2261
30' 30% DC 200 on chrom PAW 80/100
Max temperature: 225 'C
Mode: constant flow

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 Nominal initial flow: 30.0 mL/min
Inlet: Front Inlet
Outlet: Front Detector
Outlet pressure: ambient

FRONT DETECTOR (TCD) BACK DETECTOR (NO DET)

Temperature: 175 'C (On)
Reference flow: 45.0 mL/min (On)
Mode: Constant makeup flow
Makeup flow: 0.0 mL/min (Off)
Makeup Gas Type: Helium
Filament: On
Negative polarity: Off

SIGNAL 1 SIGNAL 2
Data rate: 5 Hz Data rate: 20 Hz
Type: front detector Type: front detector
Save Data: On Save Data: Off
Zero: 0.0 (Off) Zero: 0.0 (Off)
Range: 0 Range: 0
Fast Peaks: Off Fast Peaks: Off
Attenuation: 0 Attenuation: 0

COLUMN COMP 1 COLUMN COMP 2

Derive from front detector Derive from front detector

THERMAL AUX 1
Use: Valve Box Heater
Description:
Initial temp: 75 'C (On)
Initial time: 0.00 min
# Rate Final temp Final time
1 0.0(Off)

VALVES POST RUN

Valve 1 Off Post Time: 0.00 min
Description: gas sampling valve

TIME TABLE

Time Specifier Parameter & Setpoint

0.01 Valve 1: On
1.30 Valve 1: Off

Procedure for a New Setup

This procedure will have to be carried out on a new GC or if new columns are installed or the present columns are re-
conditioned. If new columns are being installed, or present columns need to be conditioned, condition columns as
indicated in the Appendix A

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Setting the backflush time

The object is to set the backflush time of Valve 1 so that any C6+ compounds are backflushed out
as the first peak. A sample containing hexane or C6+ must be used to set up the valve timing. A
suitable sample is P/N 5080-8756 from Agilent Technologies.

1. Clear the run table of any entries and then enter the following into the run table.

Valve 1 ON Time 0.05

Valve 1 OFF Time 1.20

2. Check that you have the following set up

Oven temp 130°C

Oven time 20 min
Oven rate 0°C/min.

3. Flush the sample loop with the sample, and press START on the GC. Allow to run for the full 20
minutes. You should get a chromatogram similar to that shown below.

25 uV
Methane

2500

2000
Air

Ethane

1500
Propane

1000
Iso-Butane
Carbon Dioxide

N-Butane

Iso-Pentane

N-Pentane

500
C6 +

0
2.5 5 7.5 10 12.5 15 17.5 20 min

Fig 2.

It is important to check that both pentane peaks are present and that there is no C6 coming out later
in the run.

If the backflush time is set too early you will see that pentane peaks are missing or not all of the
pentane is present. This situation is shown in Fig 3, where a backflush time of 0.70 minutes was
used.

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If the backflush time is set too late, you will see that the C6 compounds come out later in the run.
The chromatogram shown in Fig 4 shows a peak at 15.1 min when a backflush time for Valve 1 was
set to 1.10 minutes.
25 uV

Methane
4500

4000

3500

3000

2500

2000
Ethane
Air

1500
Propane
C5 and C6

Carbon Dioxide

Iso-Butane

N-Butane
1000

500

0
2 4 6 8 10 12 14 16 min

Fig 3. Backflush too early

25 uV
Methane

2500

2000
Air

Ethane

1500
Propane

1000
Iso-Butane

N-Butane

Iso-Pentane

N-Pentane

500
C6

0
5 10 15 20 25 30 min

Fig 4. Backflush too late

The ideal time is found by increasing the backflush time of Valve 1 in 0.10 increments until the C6
peak starts to appear as shown in Fig 4. When you have found this time, decrement the backflush

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time in 0.05 decrements until this peak no longer appears. Now set the backflush time to 0.10
minutes earlier. In the example shown in Fig 4, the backflush time was 1.10 minutes. Decrementing
the time to 1.05 minutes resulted in the C6 peak disappearing. Therefore the ideal time will be 1.05 –
0.10 = 0.95 minutes.

Calibration

Connect up a calibration gas to the GC, purge the sample loop with the calibration gas and allow the
pressure in the loop to come down to atmospheric pressure before starting the run. At the end of the
run, calibrate the GC.

Tips on running the analyzer.

Sample introduction

To get reproducible results, do NOT start the GC when sample is flowing through the sample loop.
Always fill the loop and wait for about 15 seconds for the pressure in the sample loop to equilibrate
to atmospheric pressure before starting the run.

To run the GC as an analyzer automatically proceed as follows.

As stated above, it is not recommended to have flow through the sample loop when injecting the
sample into the GC. You will need a way to control the sample gas. One way is to use an external
solenoid valve controlled by the GC. The pressure of the sample to the valve should be in the 5 to
10 psi range (35 to 70 Kilopascals). The valve should be an ON/OFF type of valve. If you wish to
control this directly from the GC it should operate at 24 Volts DC and with a power rating of no more
than 1.8 watts.

Agilent cable P/N G1530-60590

Connect to
EVENT socket

White Black

Sample vent line

6890 GC
Sample in 24 V Solenoid
at 5-10 psi valve 1.8 W

The 6890 has the possibility to control 8 valves. Four of these, Valve 1 to Valve 4 are ‘internal’
valves and are used to control the valves installed on top of your instrument. The other 4 valve

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controls are available at the rear of the GC through the EVENT socket. Valve 5 and Valve 6 are 24
Volt outputs (1.8 watts ). Valve 7 and Valve 8 are contact closures. As shown on the diagram, the
solenoid valve would be controlled by the Valve 6 command.

To start the GC automatically, one Valve MUST be defined as a “Gas Sampling valve”. This can be
the actual valve that injects the sample. However, when this valve is chosen as the gas sampling
valve, you will not see ANY entries for this valve in the run table. It has been found easier to
configure all valves used in the analysis as “Switching” valves, and to define an unused valve
(dummy) as the gas sampling valve. It will far easier to change times in the timetable, especially if
the injection valve is a 10 port valve with backflush or sequence reversal.

The picture below shows a screen shot of the valve configuration screen where:

V1 is the switching valve used for this analysis

V5 is the “dummy” gas sample valve
V6 is used for the solenoid valve

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Conditioning the columns.

Due to the high percentage of liquid phase used with these columns, it is advised to condition the
columns disconnected from the detector.

The columns should be heated to 250°C for 12 hours with a flow of 30ml/min of carrier gas.

If the columns are conditioned in this GC, be careful that the valve box containing the valve does not
go above 200°C, other wise permanent damage may be done to the valve.

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