Astm D482 19
Astm D482 19
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
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.
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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
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.