ASTM D4952-12
(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 − 12
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* or both is indicated by discoloration of the sulfur floating at the
oil-water interface or by discoloration of either of the phases.
1.1 Thistestmethodcoversandisintendedprimarilyforthe
detection of mercaptans in motor fuel, kerosine, and similar
4. Significance and Use
petroleumproducts.Thismethodmayalsoprovideinformation
4.1 Sulfur present as mercaptans or as hydrogen sulfide in
onhydrogensulfideandelementalsulfurthatmaybepresentin
these sample types. distillate fuels and solvents can attack many metallic and
non-metallic materials in fuel and other distribution systems.A
1.2 The values stated in SI units are to be regarded as
negative result in the doctor test ensures that the concentration
standard. No other units of measurement are included in this
of these compounds is insufficient to cause such problems in
standard.
normal use.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Interferences
responsibility of the user of this standard to establish appro-
5.1 This test cannot be used if there are more than trace
priate safety and health practices and determine the applica-
amounts of peroxides in the test sample. Peroxides can give a
bility of regulatory limitations prior to use.
false positive results where mercaptans are at low level or not
4
even present.
2. Referenced Documents
2
5.2 To check if peroxides are present in sufficient concen-
2.1 ASTM Standards:
tration to invalidate the test, shake 10 6 0.5 mL of a fresh
D1193 Specification for Reagent Water
portion of the sample with approximately 2 mL of the
D3227 Test Method for (Thiol Mercaptan) Sulfur in
potassium iodide solution, add two drops of the acetic acid
Gasoline, Kerosine,Aviation Turbine, and Distillate Fuels
solution, and two drops of the starch solution. If the aqueous
(Potentiometric Method)
3
layer turns a blue color, this confirms the presence of peroxides
2.2 Energy Institute Standards:
in sufficient quantity to invalidate the test, and the test on this
IP30 DetectionofMercaptans,HydrogenSulfide,Elemental
sample should be discontinued. Proceed in accordance with
Sulfur, and Peroxides – Doctor Test Method
5.4.
3. Summary of Test Method
5.3 Alternatively, one may choose to perform a preliminary
Doctor Test. If a brown precipitate slowly forms, peroxide is
3.1 The sample is shaken with sodium plumbite solution, a
small quantity of powdered sulfur added, and the mixture probably present. Proceed in accordance with 5.2 to confirm
presence of peroxides at sufficient quantity to invalidate the
shaken again. The presence of mercaptans or hydrogen sulfide
test.
5.4 If interference from peroxides is confirmed, proceed to
1
This test method is under the jurisdiction of ASTM Committee D02 on
re-sample and retest. Ensure that sampling and handling
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
procedures for the new sample prevent UV light exposures as
Current edition approved April 15, 2012. Published June 2012. Originally
prescribedin7.1.Noneofthenormalrefineryunitsorblending
approved in 1989. Last previous edition approved in 2009 as D4952–09. DOI:
processes producing spark ignition motor fuels are known to
10.1520/D4952-12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or create peroxides under normal operating conditions.
contact ASTM 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 4
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, Brooks, B. T., “Sodium Plumbite or Doctor Test of Gasolines,” Industrial and
U.K., http://www.energyinst.org. Engineering Chemistry, Vol 16, No. 6, June 1924, p. 588.
*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
1
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D4952 − 12
6. Reagents and Materials bottles to wrap them in foil or place in a light-tight box to
prevent UV light exposure.
6.1 Purity of Reagents—Reagent grade chemicals shall be
used in al
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
Designation:D4952–09 Designation:D4952–12
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*
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:
D1193 Specification for Reagent Water
D3227 Test Method for (Thiol Mercaptan) Sulfur in Gasoline, Kerosine,Aviation Turbine, and Distillate Fuels (Potentiometric
Method)
3
2.2 Energy Institute Standards:
IP 30 Detection of Mercaptans, Hydrogen Sulfide, Elemental Sulfur, and Peroxides – Doctor Test 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. Interferences
5.1 This test cannot be used if there are more than trace amounts of peroxides in the test sample. Peroxides can give a false
4
positive results where mercaptans are at low level or not even present.
5.2 To check if peroxides are present in sufficient concentration to invalidate the test, shake 10 6 0.5 mL of a fresh portion of
the sample with approximately 2 mL of the potassium iodide solution, add two drops of the acetic acid solution, and two drops
of the starch solution. If the aqueous layer turns a blue color, this confirms the presence of peroxides in sufficient quantity to
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 April 15, 2009.2012. Published May 2009.June 2012. Originally approved in 1989. Last previous edition approved in 20072009as
D4952–02(2007).D4952–09. DOI: 10.1520/D4952-09.10.1520/D4952-12.
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.
3
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K., http://www.energyinst.org.
4
Brooks, B. T., “Sodium Plumbite or Doctor Test of Gasolines,” Industrial and Engineering Chemistry, Vol 16, No. 6, June 1924, p. 588.
*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.
1
---------------------- Page: 1 ----------------------
D4952–12
invalidate the test, and the test on this sample should be discontinued. Proceed in accordance with 5.4.
5.3 Alternatively, one may cho
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