ASTM D4929-04

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An American National Standard
Designation:D4929–04
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. Scope* D 6299 Practice for Applying Statistical Quality Assurance
Techniques to Evaluate Analytical Measurement System
1.1 These test methods cover the determination of organic
Performance
chloride (above 1 µg/g organically-bound chlorine) in crude
oils, using either distillation and sodium biphenyl reduction or
3. Summary of Test Method
distillation and microcoulometry.
3.1 A crude oil distillation is performed to obtain the
1.2 These test methods involve the distillation of crude oil
naphtha cut at 204°C (400°F). The distillation method was
test specimens to obtain a naphtha fraction prior to chloride
adapted from Test Method D86 for the distillation of petro-
determination. The chloride content of the naphtha fraction of
leum products. The naphtha cut is washed with caustic,
the whole crude oil can thereby be obtained. See Section 5
repeatedly when necessary, until all hydrogen sulfide is re-
regarding potential interferences.
moved. The naphtha cut, free of hydrogen sulfide, is then
1.3 Test Method A covers the determination of organic
washed with water, repeatedly when necessary, to remove
chloride in the washed naphtha fraction of crude oil by sodium
inorganic halides (chlorides).
biphenyl reduction followed by potentiometric titration.
3.2 There are two alternative test methods for determination
1.4 Test Method B covers the determination of organic
of the organic chloride in the washed naphtha fraction, as
chloride in the washed naphtha fraction of crude oil by
follows.
oxidative combustion followed by microcoulometric titration.
3.2.1 Test Method A, Sodium Biphenyl Reduction and
1.5 Values expressed in acceptable SI units are to regarded
Potentiometry—The washed naphtha fraction of a crude oil
as the standard. The preferred concentration units are micro-
specimen is weighed and transferred to a separatory funnel
grams of chloride per gram of sample.
containing sodium biphenyl reagent in toluene. The reagent is
1.6 This standard does not purport to address all of the
an addition compound of sodium and biphenyl in ethylene
safety concerns, if any, associated with its use. It is the
glycol dimethyl ether. The free radical nature of this reagent
responsibility of the user of this standard to establish appro-
promotes very rapid conversion of the organic halogen to
priate safety and health practices and determine the applica-
inorganic halide. In effect this reagent solubilizes metallic
bility of regulatory limitations prior to use.
sodium in organic compounds. The excess reagent is decom-
2. Referenced Documents posed, the mixture acidified, and the phases separated. The
2
aqueous phase is evaporated to 25 to 30 mL, acetone is added,
2.1 ASTM Standards:
and the solution titrated potentiometrically.
D 86 Test Method for Distillation of Petroleum Products at
3.2.2 Test Method B, Combustion and Microcoulometry—
Atmospheric Pressure
Thewashednaphthafractionofacrudeoilspecimenisinjected
D 1193 Specification for Reagent Water
intoaflowingstreamofgascontainingabout80 %oxygenand
D 4057 Practice for Manual Sampling of Petroleum and
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
800°C.The chlorine is converted to chloride and oxychlorides,
Petroleum Products
which then flow into a titration cell where they react with the
silver ions in the titration cell. The silver ions thus consumed
1
These test methods are under the jurisdiction of ASTM Committee D02 on
are coulometrically replaced. The total current required to
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
replace the silver ions is a measure of the chlorine present in
D02.03 on Elemental Analysis.
the injected samples.
Current edition approved Nov. 1, 2004. Published November 2004. Originally
e1
3.2.3 The reaction occurring in the titration cell as chloride
approved in 1989. Last previous edition approved in 1999 as D 4929–99 .
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
enters is as follows:
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2 1
Standards volume information, refer to the standard’s Document Summary page on Cl 1 Ag → AgCl ~s! (1)
the ASTM website.
*A Summary of Ch
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