ASTM D482-19

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: D482 − 13 D482 − 19
Designation: 4/96
Standard Test Method for
Ash from Petroleum Products
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*
1.1 This test method covers the determination of ash in the range 0.001–0.180 mass %, 0.010 % to 0.180 % by mass, from
distillate and residual fuels, gas turbine fuels, crude oils, lubricating oils, waxes, and other petroleum products, in which any
ash-forming materials present are normally considered to be undesirable impurities or contaminants (Note 1). The test method is
limited to petroleum products which are free from added ash-forming additives, including certain phosphorus compounds (Note
2).
NOTE 1—In certain types of samples, all of the ash-forming metals are not retained quantitatively in the ash. This is particularly true of distillate oils,
which require a special ash procedure in order to retain metals quantitatively.
NOTE 2—This test method is not intended for the analysis of unused lubricating oils containing additives; for such samples use Test Method D874.
Neither is it intended for the analysis of lubricating oils containing lead nor for used engine crankcase oils.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
The preferred expression of the property is mass %.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 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.
2. Referenced Documents
2.1 ASTM Standards:
D874 Test Method for Sulfated Ash from Lubricating Oils and Additives
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4928 Test Method for Water in Crude Oils by Coulometric Karl Fischer Titration
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6792 Practice for Quality Management Systems in Petroleum Products, Liquid Fuels, and Lubricants Testing Laboratories
3. Summary of Test Method
3.1 The sample contained in a suitable vessel is ignited and allowed to burn until only ash and carbon remain. The carbonaceous
residue is reduced to an ash by heating in a muffle furnace at 775°C,775 °C, cooled and weighed.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved June 15, 2013Nov. 1, 2019. Published August 2013December 2019. Originally approved in 1938. Last previous edition approved in 20122013
as D482 – 12.D482 – 13. DOI: 10.1520/D0482-13.10.1520/D0482-19.
In the IP, this test method is under the jurisdiction of the Standardization Committee. This test method was adopted as a joint ASTM-IP standard in 1965.
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
D482 − 19
4. Significance and Use
4.1 Knowledge of the amount of ash-forming material present in a product can provide information as to whether or 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 , Crucible, made of platinum, silica, or porcelain, of a capacity of 5050 mL to 150 mL.
150 mL.
NOTE 3—Alumina vessels may be used where appropriate. The use of vessels that are not made of platinum may contaminate the ash.
5.2 Electric Muffle Furnace, capable of maintaining a temperature of 775775 °C 6 25°C25 °C and preferably having suitable
apertures at the front and rear so as to allow a slow natural draught of air to pass through or a programmable furnace controlling
both temperature and air flow is suitable.
5.3 Meeker Gas Burner, or equivalent.
5.4 Mechanical Shaker.
5.5 Filter Paper.
6. Reagents
6.1 Propan-2-ol—(Warning—Flammable, can be explosive when evaporated to or near dryness.)
6.2 Toluene—(Warning—Flammable, toxic.)
6.3 Quality Control (QC) Samples , Samples, preferably are portions of one or more liquid petroleum materials that are stable
and representative of the samples of interest. These QC samples can be used to check the validity of the testing process as described
in Section 11.
7. Sampling
7.1 Obtain samples in accordance with the instructions in Practice D4057 or D4177. 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 representative
of the larger portion. Vigorous shaking can be necessary.
8. Procedure
8.1 Heat the evaporating dish or crucible that is to be used for the test at 700700 °C to 800°C800 °C for a minimum of 10 min.
10 min. Cool to room temperature in a suitable container, and weigh to the nearest 0.1 mg. 0.1 mg.
NOTE 4—The container in which the dish or crucible is cooled can be a desiccator not containing a desiccating agent. In addition, all weighings of the
crucibles should be performed as soon as the crucibles have cooled. If it should be necessary that the crucibles remain in the desiccator for a longer period,
then all subsequent weighings should be made after allowing the crucibles and contents to remain in the desiccator for the same length of time.
8.2 When the sample is sufficiently mobile, mix thoroughly before weighing. The mixing is necessary to distribute catalyst fines
and other particulate material throughout the sample. Satisfactory mixing can usually be achieved by 10 min of manual shaking
or 10 min using a mechanical shaker. Examine the sample for homogeneity before proceeding with 8.3. Continue mixing the
sample if it is not homogeneous.
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 device is described in Annex A1 of Test Methods D4928.
8.2.2 When the sample cannot be satisfactorily homogenized, reject the sample and acquire a new sample.
8.2.3 When the sample is viscous or solid at room temperature, heat the container carefully until the sample is entirely liquid
and mix carefully. An oven at an appropriate temperature can be used.
8.2.4 The sample can contain water. After heating in an oven, the water can boil causing splattering or foaming. The operator
shall proceed cautiously with the heating step, wearing appropriate personnel protective equipment, such as safety goggles and
gloves. Mixing this type of sample shall be done carefully. Stirring, rather than shaking, is an option.
8.3 The quantity of test specimen taken for testing will depend upon the ash content expected in the sample. Refer to Table 1.
The weighing procedure will also depend upon whether the sample requires heating or not, and whether more than one portion
has to be weighed.
8.4 Using a top-loading balance, weigh into the dish or 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 specimen used in the analysis at ambient temperature. One way to do this is
to take the difference between the initial and final masses of the sample container weighed at ambient temperatures. If one weighing
is sufficient, as determined from Table 1, or experience, proceed with steps 8.6 – 8.11.
8.5 If more than one addition of test
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