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: D482 − 19

Designation: 4/96

Standard Test Method for

Ash from Petroleum Products1
This standard is issued under the fixed designation D482; 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* 2. Referenced Documents

1.1 This test method covers the determination of ash in the 2.1 ASTM Standards:2
range 0.010 % to 0.180 % by mass, from distillate and residual D874 Test Method for Sulfated Ash from Lubricating Oils
fuels, gas turbine fuels, crude oils, lubricating oils, waxes, and and Additives
other petroleum products, in which any ash-forming materials D4057 Practice for Manual Sampling of Petroleum and
present are normally considered to be undesirable impurities or Petroleum Products
contaminants (Note 1). The test method is limited to petroleum D4177 Practice for Automatic Sampling of Petroleum and
products which are free from added ash-forming additives, Petroleum Products
including certain phosphorus compounds (Note 2). D4928 Test Method for Water in Crude Oils by Coulometric
Karl Fischer Titration
NOTE 1—In certain types of samples, all of the ash-forming metals are D6299 Practice for Applying Statistical Quality Assurance
not retained quantitatively in the ash. This is particularly true of distillate and Control Charting Techniques to Evaluate Analytical
oils, which require a special ash procedure in order to retain metals
quantitatively.
Measurement System Performance
NOTE 2—This test method is not intended for the analysis of unused
D6792 Practice for Quality Management Systems in Petro-
lubricating oils containing additives; for such samples use Test Method leum Products, Liquid Fuels, and Lubricants Testing
D874. Neither is it intended for the analysis of lubricating oils containing Laboratories
lead nor for used engine crankcase oils.
3. Summary of Test Method
1.2 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information 3.1 The sample contained in a suitable vessel is ignited and
only. The preferred expression of the property is mass %. allowed to burn until only ash and carbon remain. The
carbonaceous residue is reduced to an ash by heating in a
1.3 This standard does not purport to address all of the muffle furnace at 775 °C, cooled and weighed.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4. Significance and Use
priate safety, health, and environmental practices and deter-
4.1 Knowledge of the amount of ash-forming material
mine the applicability of regulatory limitations prior to use.
present in a product can provide information as to whether or
1.4 This international standard was developed in accor- not the product is suitable for use in a given application. Ash
dance with internationally recognized principles on standard- can result from oil or water-soluble metallic compounds or
ization established in the Decision on Principles for the from extraneous solids such as dirt and rust.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical 5. Apparatus
Barriers to Trade (TBT) Committee.
5.1 Evaporating Dish or Crucible, made of platinum, silica,
or porcelain, of a capacity of 50 mL to 150 mL.
1
NOTE 3—Alumina vessels may be used where appropriate. The use of
This test method is under the jurisdiction of ASTM Committee D02 on
vessels that are not made of platinum may contaminate the ash.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved Nov. 1, 2019. Published December 2019. Originally
2
approved in 1938. Last previous edition approved in 2013 as D482 – 13. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D0482-19. contact ASTM Customer Service at service@astm.org. 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. This test method was adopted as a joint ASTM-IP standard in 1965. 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

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 D482 − 19
5.2 Electric Muffle Furnace, capable of maintaining a tem- 8.2.4 The sample can contain water. After heating in an
perature of 775 °C 6 25 °C and preferably having suitable oven, the water can boil causing splattering or foaming. The
apertures at the front and rear so as to allow a slow natural operator shall proceed cautiously with the heating step, wear-
draught of air to pass through or a programmable furnace ing appropriate personnel protective equipment, such as safety
controlling both temperature and air flow is suitable. goggles and gloves. Mixing this type of sample shall be done
5.3 Meeker Gas Burner, or equivalent. carefully. Stirring, rather than shaking, is an option.
5.4 Mechanical Shaker. 8.3 The quantity of test specimen taken for testing will
depend upon the ash content expected in the sample. Refer to
5.5 Filter Paper. Table 1. The weighing procedure will also depend upon
whether the sample requires heating or not, and whether more
6. Reagents than one portion has to be weighed.
6.1 Propan-2-ol—(Warning—Flammable, can be explosive 8.4 Using a top-loading balance, weigh into the dish or
when evaporated to or near dryness.) crucible sufficient test specimen to the nearest 0.1 g to yield no
6.2 Toluene—(Warning—Flammable, toxic.) more than 20 mg of ash. Determine the mass of the test
specimen used in the analysis at ambient temperature. One way
6.3 Quality Control (QC) Samples, preferably are portions
to do this is to take the difference between the initial and final
of one or more liquid petroleum materials that are stable and
masses of the sample container weighed at ambient tempera-
representative of the samples of interest. These QC samples
tures. If one weighing is sufficient, as determined from Table 1,
can be used to check the validity of the testing process as
or experience, proceed with steps 8.6 – 8.11.
described in Section 11.
8.5 If more than one addition of test specimen is required,
7. Sampling proceed only through 8.6 (noting 8.6.1 and 8.7) and allow the
dish or crucible to cool to ambient temperature before adding
7.1 Obtain samples in accordance with the instructions in more sample as outlined in 8.4. Proceed with steps 8.6 – 8.11.
Practice D4057 or D4177. Before transferring the portion of
the sample to be ashed to the evaporating dish or crucible, take 8.6 Carefully heat the dish or crucible with a Meeker burner
particular care to ensure that the portion taken is truly or equivalent until the contents can be ignited by the flame.
representative of the larger portion. Vigorous shaking can be Maintain the dish or crucible at such a temperature that the
necessary. sample continues to burn at a uniform and moderate rate
leaving only a carbonaceous residue when the burning ceases.
8. Procedure A hot plate can be used at this stage.
8.6.1 The test sample may contain water that can cause
8.1 Heat the evaporating dish or crucible that is to be used spattering. The operator shall heat the test portion cautiously
for the test at 700 °C to 800 °C for a minimum of 10 min. Cool while wearing appropriate personnel protective equipment,
to room temperature in a suitable container, and weigh to the such as safety goggles and gloves. If spattering is very severe,
nearest 0.1 mg. so that material escapes the confines of the dish or the crucible,
NOTE 4—The container in which the dish or crucible is cooled can be discard the test portion. If the first test portion is discarded, add
a desiccator not containing a desiccating agent. In addition, all weighings 2 mL 6 1 mL of propan-2-ol (Warning—Flammable) to a
of the crucibles should be performed as soon as the crucibles have cooled. second test portion while stirring with a glass rod and warming
If it should be necessary that the crucibles remain in the desiccator for a
the test portion gently to liquefy if it is solid or near solid.
longer period, then all subsequent weighings should be made after
allowing the crucibles and contents to remain in the desiccator for the Proceed as described in 8.6. If this is unsuccessful, repeat on a
same length of time. third test portion using a 10 mL 6 1 mL mixture of 50 % 6 5
8.2 When the sample is sufficiently mobile, mix thoroughly % by volume toluene (Warning— Flammable. Vapor harmful)
before weighing. The mixing is necessary to distribute catalyst and 50 % 6 5 % by volume of propan-2-ol. In either case, any
fines and other particulate material throughout the sample. test specimen that adheres to the glass rod can be returned to
Satisfactory mixing can usually be achieved by 10 min of the dish using a strip of ashless filter paper. Continue burning
manual shaking or 10 min using a mechanical shaker. Examine as outlined in 8.6.
the sample for homogeneity before proceeding with 8.3. 8.7 Vigilance by the operator is mandatory; burning samples
Continue mixing the sample if it is not homogeneous. shall never be left unattended.
8.2.1 When it is evident that the sample is not homogenized
after repeated mixings, or there is a reasonable doubt, a
non-aerating, high-speed shear mixer can be used. Such a TABLE 1 Test Specimen Mass versus Ash
device is described in Annex A1 of Test Methods D4928. Test Specimen,
Expected Ash, mass % Ash Mass, mg
mass, g
8.2.2 When the sample cannot be satisfactorily
0.18 11 20
homogenized, reject the sample and acquire a new sample. 0.10 20 20
8.2.3 When the sample is viscous or solid at room 0.05 40 20
temperature, heat the container carefully until the sample is 0.04 50 20
0.02 100 20
entirely liquid and mix carefully. An oven at an appropriate 0.01 100 10
temperature can be used.

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 D482 − 19
8.8 Some test specimens will require extra heating after the 11. Quality Control:
burning has ceased, particularly heavy samples such as marine 11.1 Confirm the performance of the instrument or the test
fuels which form crusts over the unburned material. The crust procedure by analyzing a QC sample (see 6.3).
can be broken with a glass rod. Any crust that adheres to the 11.1.1 When QC/Quality Assurance (QA) protocols are
glass rod can be returned to the dish using a strip of ashless already established in the testing facility, these may be used to
filter paper. Burn the remaining test specimen. confirm the reliability of the test result.
8.9 The heavier material tends to foam, therefore the opera- 11.1.2 When there is no QC/QA protocol established in the
tor shall exercise considerable care. Overheating shall be testing facility, Appendix X1 can be used as the QC/QA
avoided so that neither the test specimen nor the dish are heated system.
to a red hot appearance, as this can result in loss of ash. 12. Precision and Bias3
Likewise, the flame shall never be higher than the rim of the
dish to avoid superheating the crust, thereby producing sparks 12.1 The precision of this test method as obtained by
that can result in considerable loss of ash. statistical examination of interlaboratory test results is as
follows:
8.10 Heat the residue in the muffle furnace at 775 °C 6 12.1.1 Repeatability—The difference between successive
25 °C until all carbonaceous material has disappeared. Cool the tests results, obtained by the same operator with the same
dish to room temperature in a suitable container (Note 4), and apparatus under constant operating conditions on identical test
weigh to the nearest 0.1 mg. material would, in the long run, in the normal and correct
8.11 Reheat the dish at 775 °C 6 25 °C for at least 20 min, operation of the test method, exceed the following values only
cool in a suitable container (Note 4), and reweigh. Repeat the in one case in twenty:
heating, cooling, and weighing process until consecutive Ash, mass % Repeatability
0.010 to 0.079 0.003
weighings differ by not more than 0.5 mg. 0.080 to 0.180 0.007
12.1.2 Reproducibility—The difference between two single
9. Calculation and independent results obtained by different operators in
9.1 Calculate the mass of the ash as a percentage of the different laboratories on identical test material would, in the
original samples as follows: long run, in the normal and correct operation of the test
method, exceed the following values only in one case in
Ash, mass % 5 ~ w/W ! 3 100 (1)
twenty:
where: Ash, mass % Reproducibility
w = mass of ash, g, and 0.010 to 0.079 0.005
0.080 to 0.180 0.024
W = mass of sample, g.
12.2 Bias—The bias of this test method cannot be deter-
10. Report mined since an appropriate standard reference material con-
taining a known level of ash in liquid petroleum hydrocarbon
10.1 Report the results as follows: is not available.
Test Specimen Mass Report
9.00 g to 39.99 g 3 decimal places 13. Keywords
40.00 g or more 3 to 4 decimal places
13.1 ash; crude oils; distillate oils; fuel oils; lubricating oils
10.2 Record the value reported as ash in accordance with
Test Method D482, stating the mass of the sample taken. 3
No ASTM Research Report is available for this standard.

APPENDIX

(Nonmandatory Information)

X1. QUALITY CONTROL

X1.1 Confirm the performance of the instrument or the test X1.3 Record the QC results and analyze by control charts or
procedure by analyzing a QC sample. other statistically equivalent techniques, to ascertain the statis-
tical control status of the total testing process (see Practices
X1.2 Prior to monitoring the measurement process, the user D6299 and D6792 and MNL 7). Any out-of-control data should
of the test method needs to determine the average value and trigger investigation for root cause(s).
control limits of the QC sample (see Practices D6299 and
D6792 and MNL 7).4 X1.4 In the absence of explicit requirements given in the
test method, the frequency of QC testing is dependent on the
4
ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis, 6th criticality of the quality being measured, the demonstrated
ed., ASTM International, W. Conshohocken, PA. stability of the testing process, and customer requirements.

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 D482 − 19
Generally, a QC sample is analyzed each testing day with X1.5 It is recommended that, if possible, the type of QC
routine samples. The QC frequency should be increased if a sample that is regularly tested be representative of the material
large number of samples are routinely analyzed. However, routinely analyzed. An ample supply of QC sample material
when it is demonstrated that the testing is under statistical should be available for the intended period of use, and must be
control, the QC testing frequency may be reduced. The QC homogenous and stable under the anticipated storage condi-
sample precision should be checked against the ASTM method tions. See Practice D6299 and D6792 and MNL 7 for further
precision to ensure data quality. guidance on QC and Control Charting techniques.

SUMMARY OF CHANGES

Subcommittee D02.03 has identified the location of selected changes to this standard since the last issue
(D482 – 13) that may impact the use of this standard. (Approved Nov. 1, 2019.)

(1) Revised subsection 1.1. (3) Revised ash mass % values in subsections 12.1.1 and
(2) Revised Table 1. 12.1.2.

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