Designation: D482 − 07

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 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 0.001–0.180 mass %, from distillate and residual fuels, D874 Test Method for Sulfated Ash from Lubricating Oils
gas turbine fuels, crude oils, lubricating oils, waxes, and other and Additives
petroleum products, in which any ash-forming materials pres- D4057 Practice for Manual Sampling of Petroleum and
ent 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
Petroleum Products
products which are free from added ash-forming additives,
D4928 Test Method for Water in Crude Oils by Coulometric
including certain phosphorus compounds (Note 2).
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 Measurement System Performance
quantitatively. D6792 Practice for Quality System in Petroleum Products
NOTE 2—This test method is not intended for the analysis of unused and Lubricants Testing Laboratories
lubricating oils containing additives; for such samples use Test Method
D874. Neither is it intended for the analysis of lubricating oils containing 3. Summary of Test Method
lead nor for used engine crankcase oils.
3.1 The sample contained in a suitable vessel is ignited and
1.2 The values stated in SI units are to be regarded as the allowed to burn until only ash and carbon remain. The
standard. The values given in parentheses are for information carbonaceous residue is reduced to an ash by heating in a
only. The preferred expression of the property is mass %. muffle furnace at 775°C, cooled and weighed.
1.3 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4.1 Knowledge of the amount of ash-forming material
priate safety and health practices and determine the applica- present in a product can provide information as to whether or
bility of regulatory limitations prior to use. not the product is suitable for use in a given application. Ash
can result from oil or water-soluble metallic compounds or
from extraneous solids such as dirt and rust.

5. Apparatus
5.1 Evaporating Dish or Crucible , made of platinum, silica,
1
or porcelain, of 90 mL minimum capacity to 120-mL maxi-
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
mum capacity.
D02.03 on Elemental Analysis.
Current edition approved Dec. 1, 2007. Published January 2008. Originally
2
approved in 1938. Last previous edition approved in 2003 as D482–03. 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 [email protected]. For Annual Book of ASTM
Committee. This test method was adopted as a joint ASTM-IP standard in 1965. Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D0482-07. the ASTM website.

*A Summary of Changes section appears at the end of this standard

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 D482 − 07
5.2 Electric Muffle Furnace, capable of maintaining a tem- 8.2.3 When the sample is viscous or solid at room tempera-
perature of 775 6 25°C and preferably having suitable ture, heat the container carefully until the sample is entirely
apertures at the front and rear so as to allow a slow natural liquid and mix carefully. An oven at an appropriate temperature
draught of air to pass through. can be used.
5.3 Meeker Gas Burner, or equivalent. 8.2.4 The sample can contain water. After heating in an
oven, the water can boil causing splattering or foaming. The
5.4 Mechanical Shaker.3 operator shall proceed cautiously with the heating step, wear-
ing appropriate personnel protective equipment, such as safety
6. Reagents goggles and gloves. Mixing this type of sample shall be done
6.1 Propan-2-ol—(Warning—Flammable, can be explosive carefully. Stirring, rather than shaking, is an option.
when evaporated to or near dryness.) 8.3 The quantity of test specimen taken for testing will
6.2 Toluene—(Warning—Flammable, toxic.) depend upon the ash content expected in the sample. Refer to
Table 1. The weighing procedure will also depend upon
6.3 Quality Control (QC) Samples , preferably are portions
whether the sample requires heating or not, and whether more
of one or more liquid petroleum materials that are stable and
than one portion has to be weighed.
representative of the samples of interest. These QC samples
can be used to check the validity of the testing process as 8.4 Using a top-loading balance, weigh into the dish or
described in Section 11. crucible sufficient test specimen to the nearest 0.1 g to yield no
more than 20 mg of ash. Determine the mass of the test
7. Sampling specimen used in the analysis at ambient temperature. One way
to do this is to take the difference between the initial and final
7.1 Obtain samples in accordance with the instructions in
masses of the sample container weighed at ambient tempera-
Practice D4057 or D4177. Before transferring the portion of
tures. If one weighing is sufficient, as determined from Table 1,
the sample to be ashed to the evaporating dish or crucible, take
or experience, proceed with steps 8.6-8.11.
particular care to ensure that the portion taken is truly
representative of the larger portion. Vigorous shaking can be 8.5 If more than one addition of test specimen is required,
necessary. 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
8. Procedure more sample as outlined in 8.4. Proceed with steps 8.6-8.11.
8.1 Heat the evaporating dish or crucible that is to be used 8.6 Carefully heat the dish or crucible with a Meeker burner
for the test at 700 to 800°C for a minimum of 10 min. Cool to or equivalent until the contents can be ignited by the flame.
room temperature in a suitable container, and weigh to the Maintain the dish or crucible at such a temperature that the
nearest 0.1 mg. sample continues to burn at a uniform and moderate rate
leaving only a carbonaceous residue when the burning ceases.
NOTE 3—The container in which the dish or crucible is cooled can be A hot plate can be used at this stage.
a desiccator not containing a desiccating agent. In addition, all weighings
of the crucibles should be performed as soon as the crucibles have cooled. 8.6.1 The test sample may contain water that can cause
If it should be necessary that the crucibles remain in the desiccator for a spattering. The operator shall heat the test portion cautiously
longer period, then all subsequent weighings should be made after while wearing appropriate personnel protective equipment,
allowing the crucibles and contents to remain in the desiccator for the such as safety goggles and gloves. If spattering is very severe,
same length of time.
so that material escapes the confines of the dish or the crucible,
8.2 When the sample is sufficiently mobile, mix thoroughly discard the test portion. If the first test portion is discarded, add
before weighing. The mixing is necessary to distribute catalyst 2 6 1 mL of propan-2-ol (Warning—Flammable) to a second
fines and other particulate material throughout the sample. test portion while stirring with a glass rod and warming the test
Satisfactory mixing can usually be achieved by 10 min of portion gently to liquefy if it is solid or near solid. Proceed as
manual shaking or 10 min using a mechanical shaker. Examine described in 8.6. If this is unsuccessful, repeat on a third test
the sample for homogeneity before proceeding with 8.3. portion using a 10 6 1 mL mixture of 50 6 5 % by volume
Continue mixing the sample if it is not homogeneous. toluene (Warning—Flammable. Vapor harmful) and 50 6 5 %
8.2.1 When it is evident that the sample is not homogenized by volume of propan-2-ol. In either case, any test specimen that
after repeated mixings, or there is a reasonable doubt, a
non-aerating, high-speed shear mixer can be used. Such a
device is described in Annex A1 of Test Methods D4928. TABLE 1 Test Specimen Mass versus Ash
8.2.2 When the sample cannot be satisfactorily homog-
Test Specimen,
enized, reject the sample and acquire a new sample. Expected Ash, mass %
mass, g
Ash Mass, mg

0.18 11 20
0.10 20 20
0.05 40 20
3
The sole source of supply of the mechanical shaker known to the committee at 0.04 50 20
this time is the Eberbach Corp., 505 S. Maple Rd., Ann Arbor, MI 48106-1024. If 0.02 100 20
you are aware of alternative suppliers, please provide this information to ASTM 0.01 100 10
International Headquarters. Your comments will receive careful consideration at a 0.001 100 1
meeting of the responsible technical committee,1 which you may attend.

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 D482 − 07
adheres to the glass rod can be returned to the dish using a strip 11. Quality Control:
of ashless filter paper. Continue burning as outlined in 8.6. 11.1 Confirm the performance of the instrument or the test
8.7 Vigilance by the operator is mandatory; burning samples procedure by analyzing a QC sample (see 6.3).
shall never be left unattended. 11.1.1 When QC/Quality Assurance (QA) protocols are
8.8 Some test specimens will require extra heating after the already established in the testing facility, these may be used to
burning has ceased, particularly heavy samples such as marine confirm the reliability of the test result.
fuels which form crusts over the unburned material. The crust 11.1.2 When there is no QC/QA protocol established in the
can be broken with a glass rod. Any crust that adheres to the testing facility, Appendix X1 can be used as the QC/QA
glass rod can be returned to the dish using a strip of ashless system.
filter paper. Burn the remaining test specimen. 12. Precision and Bias4
8.9 The heavier material tends to foam, therefore the opera- 12.1 The precision of this test method as obtained by
tor shall exercise considerable care. Overheating shall be statistical examination of interlaboratory test results is as
avoided so that neither the test specimen nor the dish are heated follows:
to a red hot appearance, as this can result in loss of ash. 12.1.1 Repeatability—The difference between successive
Likewise, the flame shall never be higher than the rim of the tests results, obtained by the same operator with the same
dish to avoid superheating the crust, thereby producing sparks apparatus under constant operating conditions on identical test
that can result in considerable loss of ash. material would, in the long run, in the normal and correct
8.10 Heat the residue in the muffle furnace at 775 6 25°C operation of the test method, exceed the following values only
until all carbonaceous material has disappeared. Cool the dish in one case in twenty:
to room temperature in a suitable container (Note 3), and weigh Ash, mass % Repeatability
to the nearest 0.1 mg.
0.001 to 0.079 0.003
8.11 Reheat the dish at 775 6 25 °C for at least 20 min, cool 0.080 to 0.180 0.007
in a suitable container (Note 3), and reweigh. Repeat the 12.1.2 Reproducibility—The difference between two single
heating, cooling, and weighing process until consecutive and independent results obtained by different operators in
weighings differ by not more than 0.5 mg. different laboratories on identical test material would, in the
9. Calculation long run, in the normal and correct operation of the test
method, exceed the following values only in one case in
9.1 Calculate the mass of the ash as a percentage of the twenty:
original samples as follows:
Ash, mass % Reproducibility
Ash, mass % 5 ~ w/W ! 3 100 (1)
0.001 to 0.079 0.005
where: 0.080 to 0.180 0.024

w = mass of ash, g, and 12.2 Bias—The bias of this test method cannot be deter-
W = mass of sample, g. mined since an appropriate standard reference material con-
taining a known level of ash in liquid petroleum hydrocarbon
10. Report is not available.
10.1 Report the results as follows:
13. Keywords
Test Specimen Mass Report 13.1 ash; crude oils; distillate oils; fuel oils; lubricating oils
9.00 to 39.99 g 3 decimal places
40.00 or more g 3 to 4 decimal places
10.2 Record the value reported as ash in accordance with
Test Method D482, stating the mass of the sample taken. 4
No ASTM Research Report is available for this standard.

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 D482 − 07
APPENDIX

(Nonmandatory Information)

X1. QUALITY CONTROL

X1.1 Confirm the performance of the instrument or the test criticality of the quality being measured, the demonstrated
procedure by analyzing a QC sample. stability of the testing process, and customer requirements.
Generally, a QC sample is analyzed each testing day with
X1.2 Prior to monitoring the measurement process, the user
routine samples. The QC frequency should be increased if a
of the test method needs to determine the average value and
large number of samples are routinely analyzed. However,
control limits of the QC sample (see Practices D6299 and
D6792 and MNL 7).5 when it is demonstrated that the testing is under statistical
control, the QC testing frequency may be reduced. The QC
X1.3 Record the QC results and analyze by control charts or sample precision should be checked against the ASTM method
other statistically equivalent techniques, to ascertain the statis- precision to ensure data quality.
tical control status of the total testing process (see Practices
D6299 and D6792 and MNL 7). Any out-of-control data should X1.5 It is recommended that, if possible, the type of QC
trigger investigation for root cause(s). sample that is regularly tested be representative of the material
routinely analyzed. An ample supply of QC sample material
X1.4 In the absence of explicit requirements given in the
should be available for the intended period of use, and must be
test method, the frequency of QC testing is dependent on the
homogenous and stable under the anticipated storage condi-
5
ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis, 6th
tions. See Practice D6299 and D6792 and MNL 7 for further
ed., ASTM International, W. Conshohocken, PA. 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
(D482–03) that may impact the use of this standard.

(1) Added Practice D6792 to X1.2, X1.3, and X1.5 and the
Referenced Documents.

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