ASTM D4952-02(2007)
(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)
SIGNIFICANCE AND USE
Sulfur present as mercaptans or as hydrogen sulfide in distillate fuels and solvents can attack many metallic and non-metallic materials in fuel and other distribution systems. A negative result in the doctor test ensures that the concentration of these compounds is insufficient to cause such problems in normal use.
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.
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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An American National Standard
Designation:D4952–02 (Reapproved 2007)
Standard Test Method for
Qualitative Analysis for Active Sulfur Species in Fuels and
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 negative result in the doctor test ensures that the concentration
of these compounds is insufficient to cause such problems in
1.1 This test method is intended primarily for the detection
normal use.
of mercaptans in motor fuel, kerosine, and similar petroleum
products. This method may also provide information on
5. Reagents and Materials
hydrogen sulfide and elemental sulfur that may be present in
5.1 Purity of Reagents—Reagent grade chemicals shall be
these sample types.
used in all tests. Unless otherwise indicated, it is intended that
1.2 The values stated in acceptable SI units are to be
all reagents conform to the specifications of the Committee on
regarded as standard.
Analytical Reagents of the American Chemical Society where
1.3 This standard does not purport to address all of the
such specifications are available. Other grades may be used,
safety concerns, if any, associated with its use. It is the
provided it is first ascertained that the reagent is of sufficiently
responsibility of the user of this standard to establish appro-
high purity to permit its use without lessening the accuracy of
priate safety and health practices and determine the applica-
the determination.
bility of regulatory limitations prior to use.
5.2 Purity of Water—Unless otherwise indicated, references
2. Referenced Documents to water shall be understood to mean reagent water as defined
by Types II or III of Specification D 1193.
2.1 ASTM Standards:
5.3 Doctor (Sodium Plumbite) Solution—(Warning—
D 1193 Specification for Reagent Water
Poisonous and suspect carcinogen.) Dissolve approximately
D 3227 Test Method for (Thiol Mercaptan) Sulfur in Gaso-
125 g of sodium hydroxide (NaOH) in 1 L of reagent water.
line, Kerosine, Aviation Turbine, and Distillate Fuels
Add 60 g of lead monoxide (PbO) and shake vigorously for 15
(Potentiometric Method)
min, or let stand with occasional shakings for at least one day.
3. Summary of Test Method Allow to settle and decant or siphon off the clear liquid. If the
solution does not settle clear, filter it through filter paper. Keep
3.1 The sample is shaken with sodium plumbite solution, a
the solution in a tightly sealed bottle and refilter before use if
small quantity of powdered sulfur added, and the mixture
not perfectly clear. As an alternative, the lab may use a
shaken again. The presence of mercaptans or hydrogen sulfide
commercially prepared solution that meets the requirements of
or both is indicated by discoloration of the sulfur floating at the
the laboratory preparation.
oil-water interface or by discoloration of either of the phases.
NOTE 1—Alternate volumes of the solution may be prepared or
4. Significance and Use
purchased, provided the final solution concentration is equivalent.
4.1 Sulfur present as mercaptans or as hydrogen sulfide in
5.4 Sulfur—Pure, sublimed, stored in a closed container.
distillate fuels and solvents can attack many metallic and
non-metallic materials in fuel and other distribution systems.A
6. Procedure
6.1 Shake vigorously together in a test tube 10 mL of the
sample being tested and 5 mL of sodium plumbite solution for
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved May 1, 2007. Published June 2007. Originally Reagent Chemicals, American Chemical Society Specifications, American
approved in 1989. Last previous edition approved in 2002 as D 4952 – 02. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Stand
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