ASTM D4952-02
(Test Method)Standard Test Method for Qualitative Analysis for Active Sulfur Species in Fuels and Solvents (Doctor Test)
Standard Test Method for Qualitative Analysis for Active Sulfur Species in Fuels and Solvents (Doctor Test)
SCOPE
1.1 This test method is intended primarily for the detection of mercaptans in motor fuel, kerosine, and similar petroleum products. This method may also provide information on hydrogen sulfide and elemental sulfur that may be present in these sample types.
1.2 The values stated in acceptable SI units are to be regarded as standard.
1.3 This standard does not purport to address all of the safety concerns, if any, 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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Please
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An American National Standard
Designation: D 4952 – 02
Standard Test Method for
Qualitative Analysis for Active Sulfur Species in Fuels and
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Solvents (Doctor Test)
This standard is issued under the fixed designation D 4952; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* 5. Reagents and Materials
1.1 This test method is intended primarily for the detection 5.1 Purity of Reagents—Reagent grade chemicals shall be
of mercaptans in motor fuel, kerosine, and similar petroleum used in all tests. Unless otherwise indicated, it is intended that
products. This method may also provide information on all reagents conform to the specifications of the Committee on
hydrogen sulfide and elemental sulfur that may be present in Analytical Reagents of the American Chemical Society where
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these sample types. such specifications are available. Other grades may be used,
1.2 The values stated in acceptable SI units are to be provided it is first ascertained that the reagent is of sufficiently
regarded as standard. high purity to permit its use without lessening the accuracy of
1.3 This standard does not purport to address all of the the determination.
safety concerns, if any, associated with its use. It is the 5.2 Purity of Water—Unless otherwise indicated, references
responsibility of the user of this standard to establish appro- to water shall be understood to mean reagent water as defined
priate safety and health practices and determine the applica- by Types II or III of Specification D 1193.
bility of regulatory limitations prior to use. 5.3 Doctor (Sodium Plumbite) Solution—(Warning—
Poisonous and suspect carcinogen.) Dissolve approximately
2. Referenced Documents
125 g of sodium hydroxide (NaOH) in 1 L of reagent water.
2.1 ASTM Standards: Add 60 g of lead monoxide (PbO) and shake vigorously for 15
2
D 1193 Specification for Reagent Water
min, or let stand with occasional shakings for at least one day.
D 3227 Test Method for Thiol Mercaptan Sulfur in Gaso- Allow to settle and decant or siphon off the clear liquid. If the
line, Kerosine, Aviation Turbine, and Distillate Fuels
solution does not settle clear, filter it through filter paper. Keep
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(Potentiometric Method) the solution in a tightly sealed bottle and refilter before use if
not perfectly clear. As an alternative, the lab may use a
3. Summary of Test Method
commercially prepared solution that meets the requirements of
3.1 The sample is shaken with sodium plumbite solution, a
the laboratory preparation.
small quantity of powdered sulfur added, and the mixture
NOTE 1—Alternate volumes of the solution may be prepared or
shaken again. The presence of mercaptans or hydrogen sulfide
purchased, provided the final solution concentration is equivalent.
or both is indicated by discoloration of the sulfur floating at the
5.4 Sulfur—Pure, sublimed, stored in a closed container.
oil-water interface or by discoloration of either of the phases.
6. Procedure
4. Significance and Use
6.1 Shake vigorously together in a test tube 10 mL of the
4.1 Sulfur present as mercaptans or as hydrogen sulfide in
sample being tested and 5 mL of sodium plumbite solution for
distillate fuels and solvents can attack many metallic and
about 15 s. Add a small amount of pure, sublimed sulfur of
non-metallic materials in fuel and other distribution systems. A
sulfur so that practically all of it floats on the interface between
negative result in the doctor test ensures that the concentration
the sample and the sodium plumbite solution after shaking.
of these compounds is insufficient to cause such problems in
Shake again for 15 s. Allow to settle and observe within 2 min.
normal use.
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This test method is under the jurisdiction of ASTM Committee D02 on
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Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Reagent Chemicals, American Chemical Society Specifications, American
D02.03 on Elemental Analysis. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved Nov. 10, 2002. Published January 2003. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
approved in 1989. Last previous edition approved in 1997 as D 4952–97. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
2
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
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Annual Book of ASTM Standards, Vol 05.01. MD.
*A Summary of Changes section appear
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