ASTM D4952-09
(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 covers and 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 SI units are to be regarded as standard. No other units of measurement are included in this 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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Designation:D4952–09
Standard Test Method for
Qualitative Analysis for Active Sulfur Species in Fuels and
1
Solvents (Doctor Test)
This standard is issued under the fixed designation D4952; 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 (´) 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* non-metallic materials in fuel and other distribution systems.A
negative result in the doctor test ensures that the concentration
1.1 Thistestmethodcoversandisintendedprimarilyforthe
of these compounds is insufficient to cause such problems in
detection of mercaptans in motor fuel, kerosine, and similar
normal use.
petroleumproducts.Thismethodmayalsoprovideinformation
onhydrogensulfideandelementalsulfurthatmaybepresentin
5. Reagents and Materials
these sample types.
5.1 Purity of Reagents—Reagent grade chemicals shall be
1.2 The values stated in SI units are to be regarded as
used in all tests. Unless otherwise indicated, it is intended that
standard. No other units of measurement are included in this
all reagents conform to the specifications of the Committee on
standard.
Analytical Reagents of the American Chemical Society where
1.3 This standard does not purport to address all of the
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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
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by Types II or III of Specification D1193.
2.1 ASTM Standards:
5.3 Doctor (Sodium Plumbite) Solution—(Warning—
D1193 Specification for Reagent Water
Poisonous and suspect carcinogen.) Dissolve approximately
D3227 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
6. Procedure
6.1 Shake vigorously together in a test tube 10 mL of the
1
This test method is under the jurisdiction of ASTM Committee D02 on
sample being tested and 5 mL of sodium plumbite solution for
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved April 15, 2009. Published May 2009. Originally
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approved in 1989. Last previous edition approved in 2007 as D4952–02(2007). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D4952-09. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
2
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
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
An American National Standard
Designation:D4952–02 (Reapproved 2007) Designation:D4952–09
Standard Test Method for
Qualitative Analysis for Active Sulfur Species in Fuels and
1
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 (´) 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
1.1Thistestmethodisintendedprimarilyforthedetectionofmercaptansinmotorfuel,kerosine,andsimilarpetroleumproducts.
This method may also provide information on hydrogen sulfide and elemental sulfur that may be present in these sample types.
1.2The values stated in acceptable SI units are to be regarded as standard. *
1.1 This test method covers and 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 SI units are to be regarded as standard. No other units of measurement are included in this 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D 3227 Test Method for (Thiol Mercaptan) Sulfur in Gasoline, Kerosine,AviationTurbine, and Distillate Fuels (Potentiometric
Method)
3. Summary of Test Method
3.1 The sample is shaken with sodium plumbite solution, a small quantity of powdered sulfur added, and the mixture shaken
again. The presence of mercaptans or hydrogen sulfide or both is indicated by discoloration of the sulfur floating at the oil-water
interface or by discoloration of either of the phases.
4. Significance and Use
4.1 Sulfurpresentasmercaptansorashydrogensulfideindistillatefuelsandsolventscanattackmanymetallicandnon-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.
5. Reagents and Materials
5.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
3
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
5.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Types II or III of Specification D 1193.
1
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 approved in 1989. Last previous edition approved in 2002 as D4952–02.
Current edition approved April 15, 2009. Published May 2009. Originally approved in 1989. Last previous edition approved in 2007 as D 4952–02(2007).
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D4952–09
5.3 Doctor (Sodium Plumbite) Solut
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