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Astm D482 19

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263 views2 pages

Astm D482 19

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Ghassan Rokan
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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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

iTeh Standards
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
D6299 Practice for Applying Statistical Quality Assurance
and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
quantitatively.
(https://standards.iteh.ai)
NOTE 2—This test method is not intended for the analysis of unused
lubricating oils containing additives; for such samples use Test Method
D6792 Practice for Quality Management Systems in Petro-
leum Products, Liquid Fuels, and Lubricants Testing
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D874. Neither is it intended for the analysis of lubricating oils containing
lead nor for used engine crankcase oils.
Laboratories

3. Summary of Test Method


1.2 The values stated in SI units are to be regarded as the
ASTM D482-19
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
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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 [email protected]. 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

1
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

iTeh Standards
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. (https://standards.iteh.ai) sample continues to burn at a uniform and moderate rate
leaving only a carbonaceous residue when the burning ceases.

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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,
ASTM
to room temperature in a suitable container, and weigh D482-19
to the such as safety goggles and gloves. If spattering is very severe,
nearest 0.1 mg.
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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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