ASTM D874-13a
(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 mass % is restricted to oils containing ashless additives. The lower limit of the test method is 0.005 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D874 − 13a 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 Department of Defense.
1. Scope* 2. Referenced Documents
2
1.1 This test method covers the determination of the sul- 2.1 ASTM Standards:
fated ash from unused lubricating oils containing additives and D482 Test Method for Ash from Petroleum Products
from additive concentrates used in compounding. These addi- D1193 Specification for Reagent Water
tives usually contain one or more of the following metals: D4057 Practice for Manual Sampling of Petroleum and
barium,calcium,magnesium,zinc,potassium,sodium,andtin. Petroleum Products
The elements sulfur, phosphorus, and chlorine can also be D4177 Practice for Automatic Sampling of Petroleum and
present in combined form. Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance
1.2 Application of this test method to sulfated ash levels
and Control Charting Techniques to Evaluate Analytical
below 0.02 mass % is restricted to oils containing ashless
Measurement System Performance
additives. The lower limit of the test method is 0.005 mass %
3
2.2 CEN Standards:
sulfated ash.
EN 14213 Heating Fuels—Fatty Acid Methyl Esters
NOTE 1—This test method is not intended for the analysis of used
(FAME)—Requirements and Test Methods
engine oils or oils containing lead. Neither is it recommended for the
EN 14214 Automotive Fuels—Fatty Acid Methyl Esters
analysis of nonadditive lubricating oils, for which Test Method D482 can
(FAME) for Diesel Engines—Requirements and Test
be used.
Methods
NOTE 2—There is evidence that magnesium does not react the same as
otheralkalimetalsinthistest.Ifmagnesiumadditivesarepresent,thedata
is interpreted with caution.
3. Terminology
NOTE 3—There is evidence that samples containing molybdenum can
3.1 Definitions:
give low results because molybdenum compounds are not fully recovered
at the temperature of ashing. 3.1.1 sulfated ash—the residue remaining after the sample
has been carbonized, and the residue subsequently treated with
1.3 Fatty acid methyl ester (FAME) conforming to EN
sulfuric acid and heated to constant weight.
14213 and EN 14214, when tested using this test method, were
shown to meet its precision.
4. Summary of Test Method
1.4 The values stated in SI units are to be regarded as
4.1 The sample is ignited and burned until only ash and
standard. No other units of measurement are included in this
carbon remain. After cooling, the residue is treated with
standard.
sulfuric acid and heated at 775°C until oxidation of carbon is
1.5 This standard does not purport to address all of the
complete. The ash is then cooled, re-treated with sulfuric acid,
safety concerns, if any, associated with its use. It is the
and heated at 775°C to constant weight.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 5. Significance and Use
bility of regulatory limitations prior to use.
5.1 The sulfated ash can be used to indicate the concentra-
tion of known metal-containing additives in new oils. When
phosphorus is absent, barium, calcium, magnesium, sodium
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
2
D02.03 on Elemental Analysis. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Sept. 1, 2013. Published September 2013. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1946. Last previous edition approved in 2013 as D874 – 13. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D0874-13A. the ASTM website.
3
In the IP, this test method is under the jurisdiction of the Standardization Available from European Committee for Standardization (CEN-CENELEC
Committee. This test method has been approved by the sponsoring committees and Management Centre), Avenue Marnix 17, B-1000, Brussels, Belgium, http://
accepted by the cooperating societies in accordance with established procedures. www.cenorm.be.
*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 ----------------------
D874 − 13a
...
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 − 13 D874 − 13a 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 Department of Defense.
1. 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 mass % is restricted to oils containing ashless additives.
The lower limit of the test method is 0.005 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 and health practices and determine the applicability of regulatory
limitations prior to use.
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:
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 Aug. 1, 2013Sept. 1, 2013. Published August 2013September 2013. Originally approved in 1946. Last previous edition approved in 20072013
as D874 – 07.D874 – 13. DOI: 10.1520/D0874-13.10.1520/D0874-13A.
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.
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.
3
Available from European Committee for Standardization (CEN-CENELEC Management Centre), Avenue Marnix 17, B-1000, Brussels, Belgium, http://www.cenorm.be.
*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 ----------------------
D874 − 13a
3.1.1 sulfated ash—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 sulfuric ac
...
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