FED-STD-791D
5. MATERIALS
5.1 CAUTION: SOME MATERIALS ARE TOXIC AND HAZARDOUS. The
chemical materials listed in this section must be handled carefully. Federal Test Method
10000, Material Handling Safety Precautions, is a reference which lists all toxic and
hazardous materials cited in FTMS 791. The synonyms, life hazard, flammability,
handling and storage precautions, emergency treatment and measures, and spill practices
of each chemical are explained.
5.2 Hexane, normal, ACS [1,3,0].
5.3 Extraction thimble (double thickness 3.3
8.0 cm).
5.4 Filter paper (Whatman No. l or equivalent).
5.5 Filter paper (Whatman No. 40 or equivalent).
5.6 Eschka's mixture - 2 parts of calcined ("light") magnesia thoroughly mixed
with one part of sodium carbonate [u,u,u].
5.7 Bromine water, saturated [4,0,0].
5.8 Barium chloride, 10% [0,0,2].
5.9 Sodium carbonate, CP [u,u,u].
5.10 Potassium carbonate, CP [u,u,u].
6. PROCEDURE
6.1 Determine the solids content of the grease as follows:
a. Dry an extraction thimble (3.3 8.0 cm) at 100C, cool in a desiccator
and weigh to the 100 C nearest tenth of a mg. Dry thimble to constant
weight. Weigh approximately 5 g of the grease to be tested into the
extraction thimble.
b. Place 200 mL of n-hexane in the flask, place the thimble containing the
grease sample in the Soxhlet extraction tube, and assemble the apparatus
as shown in Figure 1.
c. By means of a hotplate bring the hexane to boiling and reflux until the
base oil has been completely extracted from the grease (see Note 1).
Complete removal of the oil may be determined by sampling small (2 mL)
quantities of hexane from the extraction tube and evaporating on a clean
evaporating dish. An oily film will remain if oil is contained in the
sample.
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