ASTM D129-18
(Test Method)Standard Test Method for Sulfur in Petroleum Products (General High Pressure Decomposition Device Method) (Withdrawn 2023)
Standard Test Method for Sulfur in Petroleum Products (General High Pressure Decomposition Device Method) (Withdrawn 2023)
ABSTRACT
This standard details the general bomb test method for determination of the amount of sulfur in lubricating oils with additives, additive concentrates, lubricating greases, and other petroleum products with low volatilities. This test method entails oxidizing samples by combustion in a bomb containing oxygen under pressure. The amount of sulfur is determined by gravimetry. Materials needed for the test include a combustion bomb, sample cup, firing wire, ignition circuit, and a cotton wicking or nylon sewing thread. All reagents, samples, and other chemicals used for the test should conform to the required concentration and purity.
SCOPE
1.1 This test method covers the determination of sulfur in petroleum products, including lubricating oils containing additives, additive concentrates, and lubricating greases that cannot be burned completely in a wick lamp. The test method is applicable to any petroleum product sufficiently low in volatility that it can be weighed accurately in an open sample boat and containing at least 0.1 % sulfur.
Note 1: This test method is not applicable to samples containing elements that give residues, other than barium sulfate, which are insoluble in dilute hydrochloric acid and would interfere in the precipitation step. These interfering elements include iron, aluminum, calcium, silicon, and lead which are sometimes present in greases, lube oil additives, or additive oils. Other acid insoluble materials that interfere are silica, molybdenum disulfide, asbestos, mica, and so forth. The test method is not applicable to used oils containing wear metals, and lead or silicates from contamination. Samples that are excluded can be analyzed by Test Method D1552.
1.2 This test method is applicable to samples with the sulfur in the range 0.09 % to 5.5 % by mass.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
WITHDRAWN RATIONALE
This test method covered the determination of sulfur in petroleum products, including lubricating oils containing additives, additive concentrates, and lubricating greases that cannot be burned completely in a wick lamp. The test method was applicable to any petroleum product sufficiently low in volatility that it can be weighed accurately in an open sample boat and containing at least 0.1 % sulfur.
During its Test Method Revision Section Meeting held in Orlando, FL on December 06, 2022; D02.03 (Elemental Analysis) test methods that were thought to be obsolete or not being used by the petroleum community were considered. D129 was identified as possibly falling into one or both categories. D129 is a jointed test method with the Energy Institute’s test method IP 61. Energy Institute members/leadership responsible for IP 61 were contacted and agreement was found. Accordingly, this standard was balloted for withdrawal with no replacement.
D129 (first approved in 1922) is a test method with a limited scope for total sulfur in the 0.09 % to 5.5 % by mass range. The summary of the test method informs that the sample is oxidized by combustion in a high pressure decomposition device containing oxygen under pressure. The sulfur, as sulfate in the high-pressure decomposition device washings, is determined gravimetrically as barium sulfate. A suitable warning is...
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D129 − 18 British Standard 4454
Designation: 61/99
Standard Test Method for
Sulfur in Petroleum Products (General High Pressure
1
Decomposition Device Method)
This standard is issued under the fixed designation D129; 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 U.S. Department of Defense.
1. Scope* mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.1 This test method covers the determination of sulfur in
petroleum products, including lubricating oils containing
2. Referenced Documents
additives, additive concentrates, and lubricating greases that
2
2.1 ASTM Standards:
cannot be burned completely in a wick lamp. The test method
D1193 Specification for Reagent Water
is applicable to any petroleum product sufficiently low in
D1552 Test Method for Sulfur in Petroleum Products by
volatility that it can be weighed accurately in an open sample
High Temperature Combustion and Infrared (IR) Detec-
boat and containing at least 0.1 % sulfur.
tion or Thermal Conductivity Detection (TCD)
NOTE 1—This test method is not applicable to samples containing
D4057 Practice for Manual Sampling of Petroleum and
elements that give residues, other than barium sulfate, which are insoluble
Petroleum Products
in dilute hydrochloric acid and would interfere in the precipitation step.
D4177 Practice for Automatic Sampling of Petroleum and
These interfering elements include iron, aluminum, calcium, silicon, and
leadwhicharesometimespresentingreases,lubeoiladditives,oradditive Petroleum Products
oils. Other acid insoluble materials that interfere are silica, molybdenum
D6299 Practice for Applying Statistical Quality Assurance
disulfide,asbestos,mica,andsoforth.Thetestmethodisnotapplicable to
and Control Charting Techniques to Evaluate Analytical
usedoilscontainingwearmetals,andleadorsilicatesfromcontamination.
Measurement System Performance
Samples that are excluded can be analyzed by Test Method D1552.
E144 Practice for Safe Use of Oxygen Combustion Vessels
1.2 This test method is applicable to samples with the sulfur
in the range 0.09 % to 5.5 % by mass.
3. Summary of Test Method
1.3 The values stated in SI units are to be regarded as
3.1 Thesampleisoxidizedbycombustioninahighpressure
standard. No other units of measurement are included in this
decomposition device containing oxygen under pressure. The
standard.
sulfur, as sulfate in the high pressure decomposition device
1.4 This standard does not purport to address all of the
washings, is determined gravimetrically as barium sulfate.
safety concerns, if any, associated with its use. It is the
3.2 (Warning—Strict adherence to all of the provisions
responsibility of the user of this standard to establish appro-
prescribed hereafter ensures against explosive rupture of the
priate safety, health, and environmental practices and deter-
high pressure decomposition device, or a blow-out, provided
mine the applicability of regulatory limitations prior to use.
the high pressure decomposition device is of proper design and
1.5 This international standard was developed in accor-
construction and in good mechanical condition. It is desirable,
dance with internationally recognized principles on standard-
however, that the high pressure decomposition device be
ization established in the Decision on Principles for the
enclosed in a shield of steel plate at least 13 mm thick, or
Development of International Standards, Guides and Recom-
equivalent protection be provided against unforeseeable con-
tingencies.)
1
This test method is under the jurisdiction of ASTM Committee D02 on
3.3 (Warning—Initial testing and periodic examination of
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
the pressure vessel is essential to ensure its fitness for service.
Subcommittee D02.03 on Elemental Analysis.
Current edition approved April 1, 2018. Published April 2018. Originally
approved in 1922. Last previous edition approved in 2013 as D129 – 13. DOI:
2
10.1520/D0129-18. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method was adopted as a joint ASTM-IP standard in 1964. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
In the IP, this test method is under the jurisdiction of the Standardization Standards volume information, refer to the stan
...
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: D129 − 13 D129 − 18 British Standard 4454
Designation: 61/99
Standard Test Method for
Sulfur in Petroleum Products (General High Pressure
1
Decomposition Device Method)
This standard is issued under the fixed designation D129; 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 U.S. Department of Defense.
1. Scope*
1.1 This test method covers the determination of sulfur in petroleum products, including lubricating oils containing additives,
additive concentrates, and lubricating greases that cannot be burned completely in a wick lamp. The test method is applicable to
any petroleum product sufficiently low in volatility that it can be weighed accurately in an open sample boat and containing at least
0.1 % sulfur.
NOTE 1—This test method is not applicable to samples containing elements that give residues, other than barium sulfate, which are insoluble in dilute
hydrochloric acid and would interfere in the precipitation step. These interfering elements include iron, aluminum, calcium, silicon, and lead which are
sometimes present in greases, lube oil additives, or additive oils. Other acid insoluble materials that interfere are silica, molybdenum disulfide, asbestos,
mica, and so forth. The test method is not applicable to used oils containing wear metals, and lead or silicates from contamination. Samples that are
excluded can be analyzed by Test Method D1552.
1.2 This test method is applicable to samples with the sulfur in the range 0.09 to 5.5 mass %.0.09 % to 5.5 % by mass.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D1552 Test Method for Sulfur in Petroleum Products by High Temperature Combustion and Infrared (IR) Detection or Thermal
Conductivity Detection (TCD)
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
E144 Practice for Safe Use of Oxygen Combustion Vessels
3. Summary of Test Method
3.1 The sample is oxidized by combustion in a high pressure decomposition device containing oxygen under pressure. The
sulfur, as sulfate in the high pressure decomposition device washings, is determined gravimetrically as barium sulfate.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved June 15, 2013April 1, 2018. Published August 2013April 2018. Originally approved in 1922. Last previous edition approved in 20112013 as
D129 – 11.D129 – 13. DOI: 10.1520/D0129-13.10.1520/D0129-18.
This test method was adopted as a joint ASTM-IP standard in 1964.
In the IP, this test method is under the jurisdiction of the Standardization Committee.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 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.
*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 ----------------------
D129 − 18
3.2 (Warning—Strict adherence to all of the pro
...
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D129 − 18 British Standard 4454
Designation: 61/99
Standard Test Method for
Sulfur in Petroleum Products (General High Pressure
1
Decomposition Device Method)
This standard is issued under the fixed designation D129; 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 U.S. Department of Defense.
1. Scope* mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.1 This test method covers the determination of sulfur in
petroleum products, including lubricating oils containing
2. Referenced Documents
additives, additive concentrates, and lubricating greases that
2
2.1 ASTM Standards:
cannot be burned completely in a wick lamp. The test method
D1193 Specification for Reagent Water
is applicable to any petroleum product sufficiently low in
D1552 Test Method for Sulfur in Petroleum Products by
volatility that it can be weighed accurately in an open sample
High Temperature Combustion and Infrared (IR) Detec-
boat and containing at least 0.1 % sulfur.
tion or Thermal Conductivity Detection (TCD)
NOTE 1—This test method is not applicable to samples containing
D4057 Practice for Manual Sampling of Petroleum and
elements that give residues, other than barium sulfate, which are insoluble
Petroleum Products
in dilute hydrochloric acid and would interfere in the precipitation step.
D4177 Practice for Automatic Sampling of Petroleum and
These interfering elements include iron, aluminum, calcium, silicon, and
lead which are sometimes present in greases, lube oil additives, or additive
Petroleum Products
oils. Other acid insoluble materials that interfere are silica, molybdenum
D6299 Practice for Applying Statistical Quality Assurance
disulfide, asbestos, mica, and so forth. The test method is not applicable to
and Control Charting Techniques to Evaluate Analytical
used oils containing wear metals, and lead or silicates from contamination.
Measurement System Performance
Samples that are excluded can be analyzed by Test Method D1552.
E144 Practice for Safe Use of Oxygen Combustion Vessels
1.2 This test method is applicable to samples with the sulfur
in the range 0.09 % to 5.5 % by mass.
3. Summary of Test Method
1.3 The values stated in SI units are to be regarded as
3.1 The sample is oxidized by combustion in a high pressure
standard. No other units of measurement are included in this
decomposition device containing oxygen under pressure. The
standard.
sulfur, as sulfate in the high pressure decomposition device
1.4 This standard does not purport to address all of the washings, is determined gravimetrically as barium sulfate.
safety concerns, if any, associated with its use. It is the
3.2 (Warning—Strict adherence to all of the provisions
responsibility of the user of this standard to establish appro-
prescribed hereafter ensures against explosive rupture of the
priate safety, health, and environmental practices and deter-
high pressure decomposition device, or a blow-out, provided
mine the applicability of regulatory limitations prior to use.
the high pressure decomposition device is of proper design and
1.5 This international standard was developed in accor-
construction and in good mechanical condition. It is desirable,
dance with internationally recognized principles on standard-
however, that the high pressure decomposition device be
ization established in the Decision on Principles for the
enclosed in a shield of steel plate at least 13 mm thick, or
Development of International Standards, Guides and Recom-
equivalent protection be provided against unforeseeable con-
tingencies.)
1
This test method is under the jurisdiction of ASTM Committee D02 on
3.3 (Warning—Initial testing and periodic examination of
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
the pressure vessel is essential to ensure its fitness for service.
Subcommittee D02.03 on Elemental Analysis.
Current edition approved April 1, 2018. Published April 2018. Originally
approved in 1922. Last previous edition approved in 2013 as D129 – 13. DOI:
2
10.1520/D0129-18. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method was adopted as a joint ASTM-IP standard in 1964. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
In the IP, this test method is under the jurisdiction of the Standardization Standards volume information, refer to the standard’s Document Summary page on
Committee. the ASTM website.
*A Summary of Changes section appears at the end of
...
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