An American National Standard

Designation: D 482 03

Designation: 4/96

Standard Test Method for

Ash from Petroleum Products1
This standard is issued under the fixed designation D 482; 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 standard has been approved for use by agencies of the Department of Defense.

1. Scope* Petroleum Products3

1.1 This test method covers the determination of ash in the D 4928 Test Methods for Water in Crude Oils by Coulom-
range 0.0010.180 mass %, from distillate and residual fuels, etric Karl Fischer Titration3
gas turbine fuels, crude oils, lubricating oils, waxes, and other D 6299 Practice for Applying Statistical Quality Assurance
petroleum products, in which any ash-forming materials Techniques to Evaluate Analytical Measurement System
present are normally considered to be undesirable impurities or Performance4
contaminants (Note 1). The test method is limited to petroleum 3. Summary of Test Method
products which are free from added ash-forming additives,
including certain phosphorus compounds (Note 2). 3.1 The sample contained in a suitable vessel is ignited and
allowed to burn until only ash and carbon remain. The
NOTE 1In certain types of samples, all of the ash-forming metals are carbonaceous residue is reduced to an ash by heating in a
not retained quantitatively in the ash. This is particularly true of distillate
muffle furnace at 775C, cooled and weighed.
oils, which require a special ash procedure in order to retain metals
quantitatively. 4. Significance and Use
NOTE 2This test method is not intended for the analysis of unused
lubricating oils containing additives; for such samples use Test Method 4.1 Knowledge of the amount of ash-forming material
D 874. Neither is it intended for the analysis of lubricating oils containing present in a product can provide information as to whether or
lead nor for used engine crankcase oils. not the product is suitable for use in a given application. Ash
1.2 SI units are regarded as the standard. The preferred can result from oil or water-soluble metallic compounds or
expression of the property is mass %. from extraneous solids such as dirt and rust.
1.3 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5.1 Evaporating Dish or Crucible, made of platinum, silica,
priate safety and health practices and determine the applica- or porcelain, of 90 mL minimum capacity to 120-mL maxi-
bility of regulatory limitations prior to use. mum capacity.
5.2 Electric Muffle Furnace, capable of maintaining a tem-
2. Referenced Documents perature of 775 6 25C and preferably having suitable
2.1 ASTM Standards: apertures at the front and rear so as to allow a slow natural
D 874 Test Method for Sulfated Ash from Lubricating Oils draught of air to pass through.
and Additives2 5.3 Meeker Gas Burner, or equivalent.
D 4057 Practice for Manual Sampling of Petroleum and 5.4 Mechanical Shaker.5
Petroleum Products3
6. Reagents
D 4177 Practice for Automatic Sampling of Petroleum and
6.1 Propan-2-ol(WarningFlammable, can be explo-
sive when evaporated to or near dryness.)
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.
4
Current edition approved May 10, 2003. Published May 2003. Originally Annual Book of ASTM Standards, Vol 05.03.
5
approved in 1938. Last previous edition approved in 2002 as D 48202. The sole source of supply of the mechanical shaker known to the committee at
In the IP, this test method is under the jurisdiction of the Standardization this time is the Eberbach Corp., 505 S. Maple Rd., Ann Arbor, MI 48106-1024. If
Committee. This test method was adopted as a joint ASTM-IP standard in 1965. you are aware of alternative suppliers, please provide this information to ASTM
2
Annual Book of ASTM Standards, Vol 05.01. International Headquarters. Your comments will receive careful consideration at a
3
Annual Book of ASTM Standards, Vol 05.02. meeting of the responsible technical committee, 1 which you may attend.

*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
D 482 03
6.2 Toluene(WarningFlammable, toxic.) TABLE 1 Test Specimen Mass versus Ash
6.3 Quality Control (QC) Samples, preferably are portions Expected Ash, mass %
Test Specimen,
Ash Mass, mg
of one or more liquid petroleum materials that are stable and mass, g

representative of the samples of interest. These QC samples 0.18 11 20

0.10 20 20
can be used to check the validity of the testing process as 0.05 40 20
described in Section 11. 0.04 50 20
0.02 100 20
7. Sampling 0.01 100 10
0.001 100 1
7.1 Obtain samples in accordance with the instructions in
Practice D 4057 or D 4177. Before transferring the portion of
the sample to be ashed to the evaporating dish or crucible, take
particular care to ensure that the portion taken is truly to do this is to take the difference between the initial and final
representative of the larger portion. Vigorous shaking can be masses of the sample container weighed at ambient tempera-
necessary. tures. If one weighing is sufficient, as determined from Table 1,
or experience, proceed with steps 8.6-8.11.
8. Procedure 8.5 If more than one addition of test specimen is required,
8.1 Heat the evaporating dish or crucible that is to be used proceed only through 8.6 (noting 8.6.1 and 8.7) and allow the
for the test at 700 to 800C for a minimum of 10 min. Cool to dish or crucible to cool to ambient temperature before adding
room temperature in a suitable container, and weigh to the more sample as outlined in 8.4. Proceed with steps 8.6-8.11.
nearest 0.1 mg. 8.6 Carefully heat the dish or crucible with a Meeker burner
or equivalent until the contents can be ignited by the flame.
NOTE 3The container in which the dish or crucible is cooled can be
a desiccator not containing a desiccating agent. In addition, all weighings Maintain the dish or crucible at such a temperature that the
of the crucibles should be performed as soon as the crucibles have cooled. sample continues to burn at a uniform and moderate rate
If it should be necessary that the crucibles remain in the desiccator for a leaving only a carbonaceous residue when the burning ceases.
longer period, then all subsequent weighings should be made after A hot plate can be used at this stage.
allowing the crucibles and contents to remain in the desiccator for the 8.6.1 The test sample may contain water that can cause
same length of time. spattering. The operator shall heat the test portion cautiously
8.2 When the sample is sufficiently mobile, mix thoroughly while wearing appropriate personnel protective equipment,
before weighing. The mixing is necessary to distribute catalyst such as safety goggles and gloves. If spattering is very severe,
fines and other particulate material throughout the sample. so that material escapes the confines of the dish or the crucible,
Satisfactory mixing can usually be achieved by 10 min of discard the test portion. If the first test portion is discarded, add
manual shaking or 10 min using a mechanical shaker. Examine 2 6 1 mL of propan-2-ol (WarningFlammable) to a second
the sample for homogeneity before proceeding with 8.3. test portion while stirring with a glass rod and warming the test
Continue mixing the sample if it is not homogeneous. portion gently to liquefy if it is solid or near solid. Proceed as
8.2.1 When it is evident that the sample is not homogenized described in 8.6. If this is unsuccessful, repeat on a third test
after repeated mixings, or there is a reasonable doubt, a portion using a 10 6 1 mL mixture of 50 6 5 % by volume
non-aerating, high-speed shear mixer can be used. Such a toluene (WarningFlammable. Vapor harmful) and 50 6 5 %
device is described in Annex A1 of Test Methods D 4928. by volume of propan-2-ol. In either case, any test specimen that
8.2.2 When the sample cannot be satisfactorily homog- adheres to the glass rod can be returned to the dish using a strip
enized, reject the sample and acquire a new sample. of ashless filter paper. Continue burning as outlined in 8.6.
8.2.3 When the sample is viscous or solid at room tempera- 8.7 Vigilance by the operator is mandatory; burning samples
ture, heat the container carefully until the sample is entirely shall never be left unattended.
liquid and mix carefully. An oven at an appropriate temperature 8.8 Some test specimens will require extra heating after the
can be used. burning has ceased, particularly heavy samples such as marine
8.2.4 The sample can contain water. After heating in an fuels which form crusts over the unburned material. The crust
oven, the water can boil causing splattering or foaming. The can be broken with a glass rod. Any crust that adheres to the
operator shall proceed cautiously with the heating step, wear- glass rod can be returned to the dish using a strip of ashless
ing appropriate personnel protective equipment, such as safety filter paper. Burn the remaining test specimen.
goggles and gloves. Mixing this type of sample shall be done 8.9 The heavier material tends to foam, therefore the opera-
carefully. Stirring, rather than shaking, is an option. tor shall exercise considerable care. Overheating shall be
8.3 The quantity of test specimen taken for testing will avoided so that neither the test specimen nor the dish are heated
depend upon the ash content expected in the sample. Refer to to a red hot appearance, as this can result in loss of ash.
Table 1. The weighing procedure will also depend upon Likewise, the flame shall never be higher than the rim of the
whether the sample requires heating or not, and whether more dish to avoid superheating the crust, thereby producing sparks
than one portion has to be weighed. that can result in considerable loss of ash.
8.4 Using a top-loading balance, weigh into the dish or 8.10 Heat the residue in the muffle furnace at 775 6 25C
crucible sufficient test specimen to the nearest 0.1 g to yield no until all carbonaceous material has disappeared. Cool the dish
more than 20 mg of ash. Determine the mass of the test to room temperature in a suitable container (Note 3), and weigh
specimen used in the analysis at ambient temperature. One way to the nearest 0.1 mg.

2
D 482 03
8.11 Reheat the dish at 775 6 25 C for at least 20 min, cool 12. Precision and Bias 6
in a suitable container (Note 3), and reweigh. Repeat the 12.1 The precision of this test method as obtained by
heating, cooling, and weighing process until consecutive statistical examination of interlaboratory test results is as
weighings differ by not more than 0.5 mg. follows:
12.1.1 RepeatabilityThe difference between successive
9. Calculation tests results, obtained by the same operator with the same
9.1 Calculate the mass of the ash as a percentage of the apparatus under constant operating conditions on identical test
original samples as follows: material would, in the long run, in the normal and correct
Ash, mass % 5 ~w/W! 3 100 (1)
operation of the test method, exceed the following values only
in one case in twenty:
where: Ash, mass % Repeatability
w = mass of ash, g, and
0.001 to 0.079 0.003
W = mass of sample, g. 0.080 to 0.180 0.007

10. Report 12.1.2 ReproducibilityThe difference between two single

and independent results obtained by different operators in
10.1 Report the results as follows: different laboratories on identical test material would, in the
long run, in the normal and correct operation of the test
Test Specimen Mass Report
9.00 to 39.99 g 3 decimal places method, exceed the following values only in one case in
40.00 or more g 3 to 4 decimal places twenty:
10.2 Record the value reported as ash in accordance with Ash, mass % Reproducibility

Test Method D 482, stating the mass of the sample taken. 0.001 to 0.079 0.005
0.080 to 0.180 0.024
11. Quality Control 12.2 BiasThe bias of this test method cannot be deter-
11.1 Confirm the performance of the instrument or the test mined since an appropriate standard reference material con-
procedure by analyzing a QC sample (see 6.3). taining a known level of ash in liquid petroleum hydrocarbon
11.1.1 When QC/Quality Assurance (QA) protocols are is not available.
already established in the testing facility, these may be used to
13. Keywords
confirm the reliability of the test result.
11.1.2 When there is no QC/QA protocol established in the 13.1 ash; crude oils; distillate oils; fuel oils; lubricating oils
testing facility, Appendix X1 can be used as the QC/QA
system. 6
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 test method, the frequency of QC testing is dependent on the
procedure by analyzing a QC sample. criticality of the quality being measured, the demonstrated
stability of the testing process, and customer requirements.
X1.2 Prior to monitoring the measurement process, the user Generally, a QC sample is analyzed each testing day with
of the test method needs to determine the average value and routine samples. The QC frequency should be increased if a
control limits of the QC sample (see Practice D 6299 and MNL large number of samples are routinely analyzed. However,
7).7 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
sample precision should be checked against the ASTM method
or other statistically equivalent techniques, to ascertain the
precision to ensure data quality.
statistical control status of the total testing process (see Practice
D 6299 and MNL 7). Any out-of-control data should trigger X1.5 It is recommended that, if possible, the type of QC
investigation for root cause(s). sample that is regularly tested be representative of the material
X1.4 In the absence of explicit requirements given in the routinely analyzed. An ample supply of QC sample material
should be available for the intended period of use, and must be
homogenous and stable under the anticipated storage condi-
7
ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis, 6th tions. See Practice D 6299 and MNL 7 for further guidance on
ed., ASTM International, W. Conshohocken, PA. QC and Control Charting techniques.

3
D 482 03

SUMMARY OF CHANGES

Subcommittee D02.03 has identified the location of selected changes to this standard since the last issue
(D 48202) that may impact the use of this standard.

(1) Updated Table 1 to correct the Test Specimen, mass, g of 0.18 to align with the calculated value determined by Eq 1.
value from 9 to 11 for an Expected Ash, mass % value

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