LICENCE

for
IP 344:1988 (R2010) Determination Of Light Hydrocarbons In Stabilized Crude Oils - Gas
Chromatography Method

Licensee: Azecolab
Date: 01-Jun-2018

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 IP 344/88
(2010)
Determination of light hydrocarbons in stabilized crude oils
— Gas chromatography method
1 Scope
This method covers the quantitative determination
of the individual hydrocarbons in stabilized crude
oils up to and including the pentanes. The hexanes
are determined as a group.
WARNING — The use of this standard may involve
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hazardous materials, operations and equipment. This
standard does not purport to address all of the
safety problems associated with its use. It is the
responsibility of the user of this standard to
establish appropriate safety and health practices and
determine the applicability of regulatory limitations
prior to use.
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2 Principle
A known amount of an internal standard, 2,2-
dimethylbutane, is added to the stabilized crude. A
sample of this mixture is introduced by syringe into
a gas chromatographic (GC) column via a pre-
column both packed with Porapak Q. The hydro-
carbons are separated individually up to 2,2-
dimethylbutane and the hexanes are recorded as a
group. The concentrations of the individual hydro-
carbons and the hexane group, based on per cent
weight, are calculated by comparing the peak areas
with that of the internal standard.
3 Reagents and materials
Use only reagents of recognised analytical grade.
3.1 Porapak Q, 80-100 mesh.
3.2 n-pentane
3.3 2,2-Dimethylbutane, 99% pure.
3.4 2,3-dimethylbutane, 95% pure.
3.5 Cyclohexane, 95% pure.
3.6 Heptane
3.7 Carrier Gas, nitrogen or helium, free from
water and hydrocarbons.
344.1
3.8 Air and hydrogen, free from water and
hydrocarbons.
4 Apparatus
4.1 Gas chromatograph, with a heated flame
ionization detector and an injection port heater
capable of maintaining a temperature of 150°C.
4.2 Integrator, an electronic integrator or
computer system is required. It should have a count
rate of not less than 1 count per microvolt second.
4.3 Recorder, a recording potentiometer for
qualitative monitoring of the chromatogram only.
4.4 Columns, a 2 m x 2,3 mm internal diameter
column packed with Porapak Q used in conjunction
with a 100 mm x 2,3 mm internal diameter
pre-column also packed with Porapak Q.
NOTE - Means may be provided for back-flushing the
pre-column, or the packing may be disposed of after a
maximum of 10 injections. The analysis column may also
be back-flushed. Suitable back-flushing systems are
shown in Annex A.
4.5 Syringes, 10 :l and 500 :l.
4.6 Glass vials, with silicone rubber seals,
preferably PTFE-coated.
5 Apparatus preparation
5.1 Column
Degrease a 2 m length of clean stainless-steel
tubing of 2,3 mm internal diameter.
5.1.1 Packing the column
5.1.1.1 Bend the column (no bend being of less
than 50 mm in diameter) so as to be suitable for
fitting into the chromatograph.
5.1.1.2 Insert a small glass wool plug into one end
of the tube and feed the Porapak Q into the other
end by means of a funnel. An even distribution of
the packing may be achieved by gently vibrating the
 LIGHT HYDROCARBONS IN CRUDE OILS BY GAS CHROMATOGRAPHY, IP 344

column whilst appplying suction. Approximately 6.4 Shake the vial vigorously for at least 1 min
2,5 g of Porapak Q are required to pack the column. to completely mix the crude and internal standard.

5.1.1.3 Pack and prepare the 100 mm pre-column
in the same manner as the main column. There will
be no need to bend the pre-column.
5.1.2 Column conditioning
Connect the pre-column and main column together
and fit into the gas chromatograph. Do not connect
the outlet end to the detector. Condition the column
until the base line drift resulting from column bleed
is less than 1% of full-scale deflection at a column
temperature of 150°C and at the working
sensitivity.
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NOTE - Crude samples should be stored in a refrigerator
before an analysis. The preparation of internal standard
blend may be done at ambient temperature, but care
should be taken to minimize loss of light ends.
7 Procedure
7.1 Inject 1 to 5:l as necessary, of the crude oil
plus internal standard on to the column. Start the
recorder and integrator at the same time as
injection.
NOTE - The sample size should be as large as possible,
consistent with the linear range of the system, in order to

NOTE - A suitable procedure for conditioning is to give a large signal-to-noise ratio.

maintain the column at 230°C for 12 h. During this time
the carrier gas should be flowing through the column but
the column should not be connected to the detector.
5.1.3 Column performance
Using the experimental conditions set out in 5.2,
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7.2 The components are identified from the
chromatogram. A typical example is given in Figure
1. Terminate the analysis after cyclohexane has
eluted. The column may then be back-flushed or the
column temperature raised to 230°C for 30 min to
remove any heavier components.

record the chromatogram of a mixture of 1% wt

each of n-pentane (3.2), 2,2-dimethylbutane (3.3),
2,3-dimethylbutane (3.4) and cyclohexane (3.5) in
heptane (3.6).
NOTE - The ratio of valley to peak height for the
dimethylbutane peaks should be less than 15%. The
response factors for pentane and cyclohexane should be
within 5% of each other. Cyclohexane should be eluted
in less than 30 min.
7.3 Measure the peak areas.
NOTE - A constant baseline is essential for accurate
quantitative work. In this method drifting of baseline may
be caused by heavy components from a previous injection
breaking through the pre-column. Other factors such as
leaks, septum and column bleed should be checked.

5.2 Chromatograph

Typical operating conditions are:

Column temperature 150°C

Injection temperature 150°C
Detector 200°C
Carrier gas 25 ml/min

6 Sample preparation

6.1 Weigh a glass vial (4.6) and cap to the

nearest 0,1 mg.

6.2 Pour approximately 10 ml of crude oil into Figure 1: Typical chromatogram

the vial, seal immediately and reweigh to the
nearest 0,1 mg.
8 Calculation
6.3 Add approximately 200 :l of 2,2-dimethyl-
butane (3.3) by syringe (4.5) through the silicone Calculate the concentration of the individual
rubber seal in the vial cap and reweigh to the hydrocarbons and the hexane group using the
nearest 0,1 mg. following equation:

344.2
 LIGHT HYDROCARBONS IN CRUDE OILS BY GAS CHROMATOGRAPHY, IP 344

⎡ Ac × Ws ⎤ correct operation of the test method, exceed the

Component, % wt = ⎢ ⎥ 100 × RF values given in Table 2 in absolute value in only one
⎣ As × Wo ⎦ case in twenty.

where 10.3 Reproducibility, R

Ac is the peak area of component;
As is the peak area of internal standard; The difference between two single and independent
Ws is the weight of internal standard; test results, obtained by different operators working
Wo is the weight of crude oil; in different laboratories on identical test material,
RF is the response factor for carbon would in the long run, in the normal and correct
number (see Table 1). operation of the test method, exceed the values
given in Table 2 in only one case in twenty.
Table 1: Response factors
Table 2: Precision
Carbon no. Response
factor Hydrocarbon Range of r R
results X
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1 1,114
2 1,047 Ethane 0,01-0,06 0,155X 0,390X

3 1,023 Propane 0,12-0,69 0,066X 0,209X

4 1,012 Iso butane 0,16-0,32 0,056X 0,148X

5 1,005 Normal butane 0,11-1,70 0,045X 0,132X

6 1,000 Iso pentane 0,15-0,96 0,047X 0,090X

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Normal pentane 0,08-1,88 0,038X 0,103X

Cyclo pentane 0,07-0,28 0,048X 0,157X
9 Expression of results
Total hexanes 1,13-5,10 0,22 0,45

Report the results for the individual hydrocarbons up

to and including cyclopentane and for the total where X is the average of the two results being
hexane group to the nearest 0,01 % wt, Method compared.
IP 344.
11 Test report
10 Precision
The test report shall contain at least the following
10.1 General information:

The precision values (as defined in IP 367) have a) a reference to this standard;
been obtained by statistical examination of
inter-laboratory results and were first published in b) the type and complete identification of the
1988. product tested;

10.2 Repeatability, r c) the result of the test (see clause 9);

The difference between two test results, obtained d) any deviation, by agreement or otherwise,
by the same operator with the same apparatus from the procedure specified;
under constant operating conditions on identical test
material would in the long run, in the normal and e) the date of the test.

344.3
 LIGHT HYDROCARBONS IN CRUDE OILS BY GAS CHROMATOGRAPHY, IP 344

Annex A
(informative)

A.1 Back-flush of column and pre-column A.2 Back-flush of pre-column only

See Figure A.2 for arrangement for back-flush of

See Figure A.1 for arrangements for back-flush of
column and pre-column. The valve and transfer lines
must be heated.
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pre-column only. The carrier gas flows at A and B
and the vent restrictor are set so that the flow
through the analysis column is the same in both
positions of the valve.

Figure A.1: Arrangement for back-flush of Figure A.2: Arrangement for back-flush of
column and pre-column pre-column only
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344.4