ASTM D4929-99e1

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An American National Standard
e1
Designation:D4929–99
Standard Test Methods for
1
Determination of Organic Chloride Content in Crude Oil
This standard is issued under the fixed designation D 4929; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1
e NOTE—The legend in 22.1.2 was corrected editorially in August 2004.
1. Scope Techniques to Evaluate Analytical Measurement System
5
Performance
1.1 These test methods cover the determination of organic
chloride (above 1 µg/g organically-bound chlorine) in crude
3. Summary of Test Methods
oils, using either distillation and sodium biphenyl reduction or
3.1 A crude oil distillation is performed to obtain the
distillation and microcoulometry.
naphtha cut at 204°C (400°F). The distillation method was
1.2 These test methods involve the distillation of crude oil
adapted from Test Method D 86 for the distillation of petro-
test specimens to obtain a naphtha fraction prior to chloride
leum products. The naphtha cut is washed with caustic,
determination. The chloride content of the naphtha fraction of
repeatedly when necessary, until all hydrogen sulfide is re-
the whole crude oil can thereby be obtained. See Section 5
moved. The naphtha cut, free of hydrogen sulfide, is then
regarding potential interferences.
washed with water, repeatedly when necessary, to remove
1.3 Test Method A covers the determination of organic
inorganic halides (chlorides).
chloride in the washed naphtha fraction of crude oil by sodium
3.2 There are two alternative test methods for determination
biphenyl reduction followed by potentiometric titration.
of the organic chloride in the washed naphtha fraction, as
1.4 Test Method B covers the determination of organic
follows.
chloride in the washed naphtha fraction of crude oil by
3.2.1 Test Method A, Sodium Biphenyl Reduction and
oxidative combustion followed by microcoulometric titration.
Potentiometry—The washed naphtha fraction of a crude oil
1.5 This standard does not purport to address all of the
specimen is weighed and transferred to a separatory funnel
safety concerns, if any, associated with its use. It is the
containing sodium biphenyl reagent in toluene. The reagent is
responsibility of the user of this standard to establish appro-
an addition compound of sodium and biphenyl in ethylene
priate safety and health practices and determine the applica-
glycol dimethyl ether. The free radical nature of this reagent
bility of regulatory limitations prior to use.
promotes very rapid conversion of the organic halogen to
1.6 Values expressed in acceptable SI units are to regarded
inorganic halide. In effect this reagent solubilizes metallic
as the standard. The preferred concentration units are micro-
sodium in organic compounds. The excess reagent is decom-
grams of chloride per gram of sample.
posed, the mixture acidified, and the phases separated. The
2. Referenced Documents aqueous phase is evaporated to 25 to 30 mL, acetone is added,
and the solution titrated potentiometrically.
2.1 ASTM Standards:
2 3.2.2 Test Method B, Combustion and Microcoulometry—
D 86 Test Method for Distillation of Petroleum Products
3
Thewashednaphthafractionofacrudeoilspecimenisinjected
D 1193 Specification for Reagent Water
into a flowing stream of gas containing about 80 % oxygen and
D 4057 Practice for Manual Sampling of Petroleum and
4
20 % inert gas, such as argon, helium, or nitrogen.The gas and
Petroleum Products
sample flow through a combustion tube maintained at about
D 4177 Practice for Automatic Sampling of Petroleum and
4
800°C.The chlorine is converted to chloride and oxychlorides,
Petroleum Products
which then flow into a titration cell where they react with the
D 6299 Practice for Applying Statistical Quality Assurance
silver ions in the titration cell. The silver ions thus consumed
are coulometrically replaced. The total current required to
replace the silver ions is a measure of the chlorine present in
1
These test methods are under the jurisdiction of ASTM Committee D02 on
the injected samples.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
3.2.3 The reaction occurring in the titration cell as chloride
D02.03 on Elemental Analysis.
Current edition approved Jan. 10, 1999. Published March 1999. Originally enters is as follows:
published as D 4929–89. Last edition D 4929–94.
2
Annual Book of ASTM Standards, Vol 05.01.
3
Annual Book of ASTM Standards, Vol 11.01.
4 5
Annual Book of ASTM Standards, Vol 05.02. Annual Book of ASTM Standards, Vol 05.03.
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