W = weight (or volume sample).
Volatile water-soluble material, if present, may be measured as water.
Report the results as the water content to the nearest 0.05% if the 2-ml receiver has been used and to the
nearest 0.1% if the 10-ml or 25-ml receiver has been used with a 100-ml or 100-gram sample.
PART C - D-473 STANDARD TEST METHOD FOR SEDIMENT IN CRUDE
OILS AND FUEL OILS BY THE EXTRACTION METHOD
Requirements and Warnings.
Toluene Precaution - Keep away from heat, sparks, and open flame. Vapor harmful. Toluene is toxic.
Additional Precaution - Care must be taken to avoid breathing the Toluene vapor and to protect the eyes.
Keep container closed. Use with adequate ventilation. Avoid prolonged or repeated contact with the
skin.
Environmental precautions for this test method are to clean up all spills immediately. Dispose of
hazardous materials and hazardous waste IAW laboratory SOP. Report all hazardous material and
hazardous waste spills immediately. Be familiar with and know the location of MSDS for all hazardous
materials present in the workplace.
Apparatus for this test method consists of extraction apparatus, extraction flask, condenser, extraction
thimble, thimble basket, water cup, and source of heat.
Sampling for this test is obtained from the Practices of D 4057 and D 4177.
Testing procedure.
For referee tests, use a new extraction thimble. For routine tests, thimbles may be reused. Before
reusing a thimble, it must be heated to a dull red heat to remove the combustible portion of the
accumulated sediment.
Before using a new thimble, rub the outside surface with fine sandpaper and remove all loosened
material with a stiff brush. Give the thimble a preliminary extraction with the toluene, allowing the solvent
to drip from the thimble for at least 1 hour. Then dry the thimble for 1 hour at a temperature of 115 to
120C; cool in a desiccator, without desiccant, for 1 hour, and weigh to the nearest 0.1 mg. Repeat this
extraction until the masses of the thimble after two successive extractions do not differ by more than 0.2
mg.
Place an estimated 10-gram test portion of the sample in the thimble immediately after the sample is
mixed. Do not attempt to adjust this estimated 10-gram portion to any exact predetermined amount.
Weigh to the nearest 0.01 gram. Place the thimble in the extraction apparatus, and extract with the hot
toluene for 30 minutes after the solvent dropping from the thimble is colorless. Ensure that the rate of
extraction is such that the surface of the mixture of oil and toluene in the thimble does not rise higher
than to within 20 mm of the top.
When testing samples have a high water content, any water in the test portion is removed as its toluene
azeotrope and is collected in the water cup, where it separates as a bottom layer. The toluene layer
overflows into the thimble. If the cup becomes full of water, allow the apparatus to cool and empty the
cup.
After the extraction is completed, dry the thimble for 1 hour at 115 to 120C; cool in a desiccator, without
desiccant, for 1 hour, and weigh to the nearest 0.2 mg.
Repeat the extraction, allowing the solvent to drip from the thimble for at least 1 hour but not longer than
1.25 hour; dry, cool, and weigh the thimble. Repeat this extraction for further 1 hour periods, if
necessary, until masses of the dried thimble plus sediment, after two successive extractions, do not differ
by more than 0.2 mg.
Calculation and reporting procedures. Calculate the mass of the sediment as a percent of the
original sample as follows:
Mass % = ____mass sediment___ x 100
original sample mass
Report the results to the nearest 0.01% as the mass percent of sediment by extraction. The test report shall
reference this Test Method D 473 as the procedure used.
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QM 5181
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