ASTM D874-00
(Test Method)Standard Test Method for Sulfated Ash from Lubricating Oils and Additives
Standard Test Method for Sulfated Ash from Lubricating Oils and Additives
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 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 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.
1.4 The values given in acceptable metric units are to be regarded as the standard.
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
An American National Standard
Designation:D874–00 British Standard 4716
Designation: 163/96
Standard Test Method for
Sulfated Ash from Lubricating Oils and Additives
This standard is issued under the fixed designation D 874; 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 (e) indicates an editorial change since the last revision or reapproval.
This test method has been approved by the sponsoring committees and accepted by the cooperating societies in accordance with
established procedures.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* 2. Referenced Documents
1.1 This test method covers the determination of the sul- 2.1 ASTM Standards:
fated ash from unused lubricating oils containing additives and D 482 Test Method for Ash from Petroleum Products
from additive concentrates used in compounding. These addi- D 1193 Specification for Reagent Water
tives usually contain one or more of the following metals: D 4057 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 D 4177 Practice for Automatic Sampling of Petroleum and
present in combined form. Petroleum Products
1.2 Application of this test method to sulfated ash levels D 6299 Practice for Applying Statistical Quality Assurance
below 0.02 mass % is restricted to oils containing ashless Techniques to Evaluate Analytical Measurement System
additives. The lower limit of the method is 0.005 mass % Performance
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 D 482 can
has been carbonized, and the residue subsequently treated with
be used.
NOTE 2—There is evidence that magnesium does not react the same as
sulfuric acid and heated to constant weight.
otheralkalimetalsinthistest.Ifmagnesiumadditivesarepresent,thedata
is interpreted with caution. 4. Summary of Test Method
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 given in SI units are to be regarded as the
complete. The ash is then cooled, re-treated with sulfuric acid,
standard.
and heated at 775°C to constant weight.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5. Significance and Use
responsibility of the user of this standard to establish appro-
5.1 The sulfated ash can be used to indicate the concentra-
priate safety and health practices and determine the applica-
tion of known metal-containing additives in new oils. When
bility of regulatory limitations prior to use.
phosphorus is absent, barium, calcium, magnesium, sodium
and potassium are converted to their sulfates and tin (stannic)
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. Annual Book of ASTM Standards, Vol 05.01.
In the IP, this method is under the jurisdiction of the Standardization Committee. Annual Book of ASTM Standards, Vol 11.01.
Current edition approved Jan. 10, 2000. Published March 2000. Originally Annual Book of ASTM Standards, Vol 05.02.
published as D 874 – 46. Last previous edition D 874 – 96. Annual Book of ASTM Standards, Vol 05.03.
*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.
D874–00
and zinc to their oxides (Note 5). Sulfur and chlorine do not 7.3 Low-Ash Mineral Oil—White oil having a sulfated ash
interfere, but when phosphorus is present with metals, it lower than the limit capable of being determined by this
remains partially or wholly in the sulfated ash as metal method.
phosphates.
NOTE 6—Determine the sulfated ash of this oil by the procedure given
in 9.1-9.11 below using 100 g of white oil weighed to the nearest 0.5 g in
NOTE 4—Since zinc sulfate slowly decomposes to its oxide at the
a 120 to 150-mL platinum dish. Deduct the sulfuric acid blank as
ignition temperature specified in the method, samples containing zinc can
described in 9.11.
give variable results unless the zinc sulfate is completely converted to the
oxide.
7.4 Sulfuric Acid (relative density 1.84)—Concentrated sul-
5.2 Because of above inter-element interferences, experi- furic acid (H SO ). (Warning—Poison. Corrosive. Strong
2 4
mentally obtained sulfated ash values may differ from sulfated oxidizer.)
ash values calculated from elemental analysis. The formation 7.5 Sulfuric Acid (1 + 1)—Prepare by slowly adding 1
ofsuchnon-sulfatedspeciesisdependentonthetemperatureof volume of concentrated sulfuric acid (relative density 1.84) to
ashing, time ashed, and the composition of metal compounds 1 volume of water with vigorous stirring. (Warning—Mixing
present in oils. Hence, sulfated ash requirement generally this acid into water generates considerable heat. When neces-
should not be used in product specifications without a clear sary, cool the solution before adding more acid. Do not allow
understanding between a buyer and a seller of the unreliability the solution to boil.)
of an ash value as an indicator of the total metallic compound 7.6 Propan-2-ol.(Warning—Flammable, can be explosive
content. when evaporated to or near dryness.)
7.7 Toluene.(Warning—Flammable, toxic.)
6. Apparatus
7.8 Quality Control (QC) Samples, preferably are portions
6.1 Evaporating Dish or Crucible; 50 to 100-mL for
of one or more liquid petroleum materials that are stable and
samplescontainingmorethan0.02mass %sulfatedash,or120
representative of the samples of interest. These QC samples
to 150-mL for samples containing less than 0.02 mass %
can be used to check the validity of the testing process as
sulfated ash, and made of porcelain, fused silica, or platinum.
described in Section 12.
(Warning—Do not use platinum when the sample is likely to
8. Sampling
contain elements such as phosphorus, which attack platinum
under the conditions of the test.) 8.1 Obtain samples in accordance with the instructions in
Practice D 4057 or D 4177. The sample shall be thoroughly
NOTE 5—For best results on samples containing less than 0.1 mass %
mixed before removal of the laboratory test portion.
sulfated ash, platinum dishes are used. The precision values shown in
Section 13 for this type of sample were so obtained.
9. Procedure
6.2 Electric Muffle Furnace—The furnace shall be capable
9.1 Select the size of the evaporating dish or crucible
of maintaining a temperature of 775 6 25°C and preferably
according to the quantity of sample necessary (see 9.3).
haveaperturesatthefrontandreartoallowaslownaturaldraft
9.2 Heat the evaporating dish or crucible that is used for the
of air to pass through the furnace.
test at 775 6 25°C for a minimum of 10 min. Cool to room
6.3 Balance, capable of weighing to 0.1 mg.
temperatureinasuitablecontainerandweightothenearest0.1
mg.
7. Reagents
NOTE 7—The container in which the dish is cooled does not contain a
7.1 Purity of Reagents—Reagent grade chemicals shall be
desiccating agent.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
9.3 Weigh into the dish a quantity of sample given as
tee onAnalytical Reagents of theAmerican Chemical Society,
follows:
where such specifications are available, or to other recognized
W 5 10/a (1)
standards for reagent chemicals. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently where:
high purity to permit its use without lessening the accuracy of W = mass of test specimen, g, and
a = expected sulfated ash, mass %.
the determination.
However,donottakeaquantityinexcessof80g.Inthecase
7.2 Purity of Water—Unless otherwise indicated, references
of lubricating oil additives yielding a sulfated ash of 2 mass %
to water shall be understood to mean reagent water defined by
or more, dilute the weighed sample in the dish with approxi-
Types II or III of Specification D 1193.
mately 10 times its weight of low-ash mineral oil.
Further discussion of these interferences can be found in Nadkarni, R. A., NOTE 8—If the amount of sulfated ash found differs from the expected
Ledesma, R. R., and Via, G. H., “Sulfated Ash TM: Limitations of Reliability and
amount by more than a factor of two, repeat the analysis with a different
Reproducibility,” SAE Technical Paper No. 952548, available from SAE, 400
weight of sample calculated from the first analysis.
Commonwealth Drive, Warrendale, PA 15096-0001, U.S.A.
9.4 Heat the dish or crucible and sample carefully until the
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
contents can be ignited with a flame. Maintain at such a
listed by the American Chemical Society, see Analar Standards for Laboratory
temperature that the sample continues to burn at a uniform and
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
modera
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.