ASTM D874-23
(Test Method)Standard Test Method for Sulfated Ash from Lubricating Oils and Additives
Standard Test Method for Sulfated Ash from Lubricating Oils and Additives
SIGNIFICANCE AND USE
5.1 The sulfated ash can be used to indicate the concentration of known metal-containing additives in new oils. When phosphorus is absent, barium, calcium, magnesium, sodium and potassium are converted to their sulfates and tin (stannic) and zinc to their oxides (Note 4). Sulfur and chlorine do not interfere, but when phosphorus is present with metals, it remains partially or wholly in the sulfated ash as metal phosphates.
Note 4: Since zinc sulfate slowly decomposes to its oxide at the ignition temperature specified in the test method, samples containing zinc can give variable results unless the zinc sulfate is completely converted to the oxide.
5.2 Because of above inter-element interferences, experimentally obtained sulfated ash values may differ from sulfated ash values calculated from elemental analysis. The formation of such non-sulfated species is dependent on the temperature of ashing, time ashed, and the composition of metal compounds present in oils. Hence, sulfated ash requirement generally should not be used in product specifications without a clear understanding between a buyer and a seller of the unreliability of an ash value as an indicator of the total metallic compound content.4
SCOPE
1.1 This test method covers the determination of the sulfated ash from unused lubricating oils containing additives and from additive concentrates used in compounding. These additives usually contain one or more of the following metals: barium, calcium, magnesium, zinc, potassium, sodium, and tin. The elements sulfur, phosphorus, and chlorine can also be present in combined form.
1.2 Application of this test method to sulfated ash levels below 0.02 % by mass is restricted to oils containing ashless additives. The lower limit of the test method is 0.005 % by mass sulfated ash.
Note 1: This test method is not intended for the analysis of used engine oils or oils containing lead. Neither is it recommended for the analysis of nonadditive lubricating oils, for which Test Method D482 can be used.
Note 2: There is evidence that magnesium does not react the same as other alkali metals in this test. If magnesium additives are present, the data is interpreted with caution.
Note 3: There is evidence that samples containing molybdenum can give low results because molybdenum compounds are not fully recovered at the temperature of ashing.
1.3 Fatty acid methyl ester (FAME) conforming to EN 14213 and EN 14214, when tested using this test method, were shown to meet its precision.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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.
1.6 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.
General Information
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Standards Content (Sample)
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: D874 − 23 British Standard 4716
Standard Test Method for
1
Sulfated Ash from Lubricating Oils and Additives
This standard is issued under the fixed designation D874; 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* Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
1.1 This test method covers the determination of the sul-
Barriers to Trade (TBT) Committee.
fated ash from unused lubricating oils containing additives and
from additive concentrates used in compounding. These addi-
2. Referenced Documents
tives usually contain one or more of the following metals:
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barium, calcium, magnesium, zinc, potassium, sodium, and tin.
2.1 ASTM Standards:
The elements sulfur, phosphorus, and chlorine can also be
D482 Test Method for Ash from Petroleum Products
present in combined form.
D1193 Specification for Reagent Water
D4057 Practice for Manual Sampling of Petroleum and
1.2 Application of this test method to sulfated ash levels
Petroleum Products
below 0.02 % by mass is restricted to oils containing ashless
D4177 Practice for Automatic Sampling of Petroleum and
additives. The lower limit of the test method is 0.005 % by
Petroleum Products
mass sulfated ash.
D6299 Practice for Applying Statistical Quality Assurance
NOTE 1—This test method is not intended for the analysis of used
and Control Charting Techniques to Evaluate Analytical
engine oils or oils containing lead. Neither is it recommended for the
Measurement System Performance
analysis of nonadditive lubricating oils, for which Test Method D482 can
3
be used.
2.2 CEN Standards:
NOTE 2—There is evidence that magnesium does not react the same as
EN 14213 Heating Fuels—Fatty Acid Methyl Esters
other alkali metals in this test. If magnesium additives are present, the data
(FAME)—Requirements and Test Methods
is interpreted with caution.
EN 14214 Automotive Fuels—Fatty Acid Methyl Esters
NOTE 3—There is evidence that samples containing molybdenum can
give low results because molybdenum compounds are not fully recovered
(FAME) for Diesel Engines—Requirements and Test
at the temperature of ashing.
Methods
1.3 Fatty acid methyl ester (FAME) conforming to
EN 14213 and EN 14214, when tested using this test method, 3. Terminology
were shown to meet its precision.
3.1 Definitions:
1.4 The values stated in SI units are to be regarded as
3.1.1 sulfated ash, n—the residue remaining after the
standard. No other units of measurement are included in this
sample has been carbonized, and the residue subsequently
standard.
treated with sulfuric acid and heated to constant weight.
1.5 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4.1 The sample is ignited and burned until only ash and
priate safety, health, and environmental practices and deter-
carbon remain. After cooling, the residue is treated with
mine the applicability of regulatory limitations prior to use.
sulfuric acid and heated at 775 °C until oxidation of carbon is
1.6 This international standard was developed in accor-
complete. The ash is then cooled, re-treated with sulfuric acid,
dance with internationally recognized principles on standard-
and heated at 775 °C to constant weight.
ization established in the Decision on Principles for the
1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee D02.03 on Elemental Analysis. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved March 1, 2023. Published April 2023. Originally the ASTM website.
3
approved in 1946. Last previous edition approved in 2018 as D874 – 13a (2018). Available from European Committee for Standardization (CEN), Avenue
DOI: 10.1520/D0874-23. Marnix 17, B-1000, Brussels, Belgium, http://www.cen.eu.
*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 19428-29
...
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: D874 − 13a (Reapproved 2018) D874 − 23 British Standard 4716
Standard Test Method for
1
Sulfated Ash from Lubricating Oils and Additives
This standard is issued under the fixed designation D874; 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 Scope*
1.1 This test method covers the determination of the sulfated ash from unused lubricating oils containing additives and from
additive concentrates used in compounding. These additives usually contain one or more of the following metals: barium, calcium,
magnesium, zinc, potassium, sodium, and tin. The elements sulfur, phosphorus, and chlorine can also be present in combined form.
1.2 Application of this test method to sulfated ash levels below 0.02 % by mass is restricted to oils containing ashless additives.
The lower limit of the test method is 0.005 % by mass sulfated ash.
NOTE 1—This test method is not intended for the analysis of used engine oils or oils containing lead. Neither is it recommended for the analysis of
nonadditive lubricating oils, for which Test Method D482 can be used.
NOTE 2—There is evidence that magnesium does not react the same as other alkali metals in this test. If magnesium additives are present, the data is
interpreted with caution.
NOTE 3—There is evidence that samples containing molybdenum can give low results because molybdenum compounds are not fully recovered at the
temperature of ashing.
1.3 Fatty acid methyl ester (FAME) conforming to EN 14213 EN 14213 and EN 14214, when tested using this test method, were
shown to meet its precision.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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.
1.6 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.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved April 1, 2018March 1, 2023. Published June 2018April 2023. Originally approved in 1946. Last previous edition approved in 20132018 as
D874 – 13a.D874 – 13a (2018). DOI: 10.1520/D0874-13AR18.10.1520/D0874-23.
In the IP, this test method is under the jurisdiction of the Standardization Committee. This test method has been approved by the sponsoring committees and accepted by
the cooperating societies in accordance with established procedures.
*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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D874 − 23
2. Referenced Documents
2
2.1 ASTM Standards:
D482 Test Method for Ash from Petroleum Products
D1193 Specification for Reagent Water
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
3
2.2 CEN Standards:
EN 14213 Heating Fuels—Fatty Acid Methyl Esters (FAME)—Requirements and Test Methods
EN 14214 Automotive Fuels—Fatty Acid Methyl Esters (FAME) for Diesel Engines—Requirements and Test Methods
3. Terminology
3.1 Definitions:
3.1.1 sulfated ash, n—the residue remaining after the sample has been carbonized, and the residue subsequently treated with
sulfuric acid and heated to constant weight.
4. Summary of Test Method
4.1 The sample is ignited and burned until only ash and carbon remain. After cooling, the residue is treated with sulfur
...
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