ASTM D129-11

Standard Test Method for Sulfur in Petroleum Products (General High Pressure Decomposition Device Method)

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 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.

General Information

• Status: Historical
• Publication Date: 30-Sep-2011
• ICS: 75.080 - Petroleum products in general
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM D129-00(2005) - Standard Test Method for Sulfur in Petroleum Products (General Bomb Method)
• Effective Date: 01-Oct-2011
• Referred By: ASTM D2140-08(2017) - Standard Practice for Calculating Carbon-Type Composition of Insulating Oils of Petroleum Origin
• Effective Date: 01-Oct-2011
• Referred By: ASTM E165/E165M-23 - Standard Practice for Liquid Penetrant Testing for General Industry
• Effective Date: 01-Oct-2011
• Referred By: ASTM D2880-23 - Standard Specification for Gas Turbine Fuel Oils
• Effective Date: 01-Oct-2011
• Referred By: ASTM D396-21 - Standard Specification for Fuel Oils
• Effective Date: 01-Oct-2011
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 01-Oct-2011
• Referred By: ASTM D7467-20a - Standard Specification for Diesel Fuel Oil, Biodiesel Blend (B6 to B20)
• Effective Date: 01-Oct-2011
• Referred By: ASTM E1210-21 - Standard Practice for Fluorescent Liquid Penetrant Testing Using the Hydrophilic Post-Emulsification Process
• Effective Date: 01-Oct-2011
• Referred By: ASTM F715-07(2023) - Standard Test Methods for Coated Fabrics Used for Oil Spill Control and Storage
• Effective Date: 01-Oct-2011
• Referred By: ASTM E1208-21 - Standard Practice for Fluorescent Liquid Penetrant Testing Using the Lipophilic Post-Emulsification Process
• Effective Date: 01-Oct-2011
• Referred By: ASTM D4809-18 - Standard Test Method for Heat of Combustion of Liquid Hydrocarbon Fuels by Bomb Calorimeter (Precision Method)
• Effective Date: 01-Oct-2011
• Referred By: ASTM D240-19 - Standard Test Method for Heat of Combustion of Liquid Hydrocarbon Fuels by Bomb Calorimeter
• Effective Date: 01-Oct-2011
• Referred By: ASTM D6823-08(2021) - Standard Specification for Commercial Boiler Fuels With Used Lubricating Oils
• Effective Date: 01-Oct-2011
• Referred By: ASTM E1219-21 - Standard Practice for Fluorescent Liquid Penetrant Testing Using the Solvent-Removable Process
• Effective Date: 01-Oct-2011
• Referred By: ASTM D4868-17 - Standard Test Method for Estimation of Net and Gross Heat of Combustion of Hydrocarbon Burner and Diesel Fuels
• Effective Date: 01-Oct-2011

Standards Content (Sample)

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 − 11
Designation:61/99 British Standard 4454
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 Department of Defense.
1. Scope* priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
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 (High-
volatility that it can be weighed accurately in an open sample
Temperature Method)
boat and containing at least 0.1 % sulfur.
D6299 Practice for Applying Statistical Quality Assurance
NOTE 1—This test method is not applicable to samples containing
and Control Charting Techniques to Evaluate Analytical
elements that give residues, other than barium sulfate, which are insoluble
Measurement System Performance
in dilute hydrochloric acid and would interfere in the precipitation step.
E144 Practice for Safe Use of Oxygen Combustion Bombs
These interfering elements include iron, aluminum, calcium, silicon, and
leadwhicharesometimespresentingreases,lubeoiladditives,oradditive
3. Summary of Test Method
oils. Other acid insoluble materials that interfere are silica, molybdenum
disulfide, asbestos, mica, and so forth.The test method is not applicable to 3.1 Thesampleisoxidizedbycombustioninahighpressure
usedoilscontainingwearmetals,andleadorsilicatesfromcontamination.
decomposition device containing oxygen under pressure. The
Samples that are excluded can be analyzed by Test Method
D1552.
sulfur, as sulfate in the high pressure decomposition device
1.2 The values stated in SI units are to be regarded as
washings, is determined gravimetrically as barium sulfate.
standard. No other units of measurement are included in this
3.2 (Warning—Strict adherence to all of the provisions
standard.
prescribed hereafter ensures against explosive rupture of the
1.3 This standard does not purport to address all of the
high pressure decomposition device, or a blow-out, provided
safety concerns, if any, associated with its use. It is the
the high pressure decomposition device is of proper design and
responsibility of the user of this standard to establish appro-
construction and in good mechanical condition. It is desirable,
however, that the high pressure decomposition device be
1
enclosed in a shield of steel plate at least 13 mm thick, or
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
equivalent protection be provided against unforeseeable con-
D02.03 on Elemental Analysis.
tingencies.)
Current edition approved Oct. 1, 2011. Published October 2011. Originally
approved in 1922. Last previous edition approved in 2005 as D129–00(2005). DOI:
2
10.1520/D0129-11. 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 [e-mail]. 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 this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D129 − 11
4. Apparatus and Materials 5.6 Oxygen, free of combustible material and sulfur com-
2
3 pounds, available at a pressure of 41 kgf/cm (40 atm).
4.1 High Pressure Decomposition Device (see Note 2), hav-
ing a capacity of not less than 300 mL, so constructed that it 5.7 Sodium Carbonate Solution(50g/L)—Dissolve135gof
will not leak during the test and that quantitative recovery of sodium carbonate decahydrate (Na CO ·10H O) or its equiva-
2 3 2
the liquids from the high pressure decomposition device may lent weight in distilled water and dilute to 1 L.
be achieved readily. The inner surface of the high pressure
5.8 White Oil, USP, or Li
...

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.
British Standard 4454
Designation:D129–00 (Reapproved 2005) Designation:D129–11
Designation: 61/99
Standard Test Method for
Sulfur in Petroleum Products (General Bomb Method)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 test method has been adopted for use by
government agencies to replace Method 5202 of Federal Test Method No. 791b
This standard has been approved for use by agencies of the 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
anypetroleumproductsufficientlylowinvolatilitythatitcanbeweighedaccuratelyinanopensampleboatandcontainingatleast
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.
1.2This 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. See 3.2 for specific precautionary directions incorporated in the test method.
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
D1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
E144 Practice for Safe Use of Oxygen Combustion Bombs
3. Summary of Test Method
3.1 The sample is oxidized by combustion in a bomb high pressure decomposition device containing oxygen under pressure.
The sulfur, as sulfate in the bomb 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 and Lubricants and is the direct responsibility of Subcommittee D02.03 on
Elemental Analysis.
Current edition approved May 1, 2005. Published May 2005. Originally approved in 1922. Last previous edition approved in 2000 as D129–00.
Current edition approved Oct. 1, 2011. Published October 2011. Originally approved in 1922. Last previous edition approved in 2005 as D129–00(2005). DOI:
10.1520/D0129-11.
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. DOI: 10.1520/D0129-00R05.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*ASummary 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 ----------------------
D129–11
3.2Warning—3.2 (Warning—Strict adherence to all of the provisions prescribed hereafter ensures against explosive r
...

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.
British Standard 4454
Designation:D129–00 (Reapproved 2005) Designation:D129–11
Designation: 61/99
Standard Test Method for
Sulfur in Petroleum Products (General Bomb Method)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 (ϵ) indicates an editorial change since the last revision or reapproval. This test method has been adopted for use by
government agencies to replace Method 5202 of Federal Test Method No. 791b
This standard has been approved for use by agencies of the 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
anypetroleumproductsufficientlylowinvolatilitythatitcanbeweighedaccuratelyinanopensampleboatandcontainingatleast
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.
1.2This 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. See 3.2 for specific precautionary directions incorporated in the test method.
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
D1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
E144 Practice for Safe Use of Oxygen Combustion Bombs
3. Summary of Test Method
3.1 The sample is oxidized by combustion in a bomb high pressure decomposition device containing oxygen under pressure.
The sulfur, as sulfate in the bomb 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 and Lubricants and is the direct responsibility of Subcommittee D02.03 on
Elemental Analysis.
Current edition approved May 1, 2005. Published May 2005. Originally approved in 1922. Last previous edition approved in 2000 as D129–00.
Current edition approved Oct. 1, 2011. Published October 2011. Originally approved in 1922. Last previous edition approved in 2005 as D129–00(2005). DOI:
10.1520/D0129-11.
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. DOI: 10.1520/D0129-00R05.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*ASummary 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 ----------------------
D129–11
3.2Warning—3.2 (Warning—Strict adherence to all of the provisions prescribed hereafter ensures against explosive r
...