ASTM D874-13
(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 5). 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.3
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 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D874 − 13 BritishStandard 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 %
sulfated ash.
3. Terminology
NOTE 1—This test method is not intended for the analysis of used
3.1 Definitions:
engine oils or oils containing lead. Neither is it recommended for the
3.1.1 sulfated ash—the residue remaining after the sample
analysis of nonadditive lubricating oils, for which Test Method D482 can
has been carbonized, and the residue subsequently treated with
be used.
sulfuric acid and heated to constant weight.
NOTE 2—There is evidence that magnesium does not react the same as
otheralkalimetalsinthistest.Ifmagnesiumadditivesarepresent,thedata
4. Summary of Test Method
is interpreted with caution.
NOTE 3—There is evidence that samples containing molybdenum can
4.1 The sample is ignited and burned until only ash and
give low results because molybdenum compounds are not fully recovered
carbon remain. After cooling, the residue is treated with
at the temperature of ashing.
sulfuric acid and heated at 775°C until oxidation of carbon is
1.3 The values stated in SI units are to be regarded as
complete. The ash is then cooled, re-treated with sulfuric acid,
standard. No other units of measurement are included in this
and heated at 775°C to constant weight.
standard.
5. Significance and Use
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5.1 The sulfated ash can be used to indicate the concentra-
responsibility of the user of this standard to establish appro-
tion of known metal-containing additives in new oils. When
priate safety and health practices and determine the applica-
phosphorus is absent, barium, calcium, magnesium, sodium
bility of regulatory limitations prior to use.
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
1
This test method is under the jurisdiction of ASTM Committee D02 on
remains partially or wholly in the sulfated ash as metal
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
phosphates.
Current edition approved Aug. 1, 2013. Published August 2013. Originally
approved in 1946. Last previous edition approved in 2007 as D874 – 07. DOI:
2
10.1520/D0874-13. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
In the IP, this test method is under the jurisdiction of the Standardization contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Committee. This test method has been approved by the sponsoring committees and Standards volume information, refer to the standard’s Document Summary page on
accepted by the cooperating societies in accordance with established procedures. 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 ----------------------
D874 − 13
NOTE 4—Since zinc sulfate slowly decomposes to its oxide at the NOTE 6—Determine the sulfated ash of this oil by the procedure given
ignition temperature specified in the test method, samples containing zinc in 9.1-9.11 below using 100 g of white oil weighed to the n
...
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 − 07 D874 − 13 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 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 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. Terminology
3.1 Definitions:
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 acid
and heated at 775°C until oxidation of carbon is complete. The ash is then cooled, re-treated with sulfuric acid, and heated at 775°C
to constant weight.
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 Nov. 1, 2007Aug. 1, 2013. Published November 2007August 2013. Originally approved in 1946. Last previous edition approved in 20062007
as D874D874 – 07.–06. DOI: 10.1520/D0874-07.10.1520/D0874-13.
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.
*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 − 13
5. 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 54). Sulfur and chlorine do not interfere, but when phosphorus is pre
...
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