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Ash, chlorine, fluorine, and sulfur |
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|  MIL-L- 24131C(SH)
Cool the Vycor dish and residue in a dessicator and weigh. Identify this residue s residue (1) and store
the Vycor dish and residue in a dessicator until ready to perform graphite content testing in accordance
with paragraph 4.4.3. From the weight of the residue in the dish and the weight of sample taken, calculate
the percent by weight of total solids using the following expression:
wt of residue (1)
x 100
Total solids, weight percent =
wt of sample
The total solids (non-volatile) content shall be in accordance with table I.
4.3.4.3. Ash, chlorine, fluorine, and sulfur. Analysis shall be made on oven dried solids obtained
by the methods of 4.3.4.2 and reported in parts per million (ppm) found in the oven dried solids.
(a)
If the supplier elects to perform the analysis on the high solids graphite mill dispersion, he
shall clean all equipment used for storage of the mill grind and for all subsequent processing
and filling to be free of all contamination, including cleaning materials. Inspections shall be
performed visually. Compounds containing boron, halides, or sulfur shall not be used in
cleaning. Equipment segregated for use in preparing this lubricant only, may be cleaned by
rinsing with isopropanol using new or segregated cleaning tools.
(b)
The supplier shall certify that the requirements of 4.3.4.3(a) have been met and that no
additions other than isopropanol have been made to the high solids graphite mill dispersion.
4.3.4.3.1 Ash shall be determined by the Loss on Ignition and Ash test of ASTM D1208 or by an
equally accurate alternate procedure which has been approved in writing.
4.3.4.3.2 Analytical procedures for chlorine and sulfur. Either spectrophotometric method (see
4.3.4.3.3) or the X-ray method (see 4.3.4.3.4) shall be used for chlorine determination. Either the X-ray
emission method or turbidimetric method (see 4.3.4.3.5) shall be used for sulfur determination. Equally
accurate alternate methods, approved in writing, may also be used.
4.3.4.3.3 Spectrophotometric method for chlorine.
(a)
Optical density shall be measured on a prepared solution against a reference solution in 5
centimeter (cm) cells by a Beckman Model "B" Spectrophotometer, or equal, at 470
millimicron (mu) and compared to the readings obtained on a series of standard solutions
containing no more than 2000 micrograms of chlorine per liter. A blank determination shall be
made in all cases.
(b)
A solution shall be prepared by fusing a 0.1-gram (g) sample with 1.0 gram of sodium
carbonate at 1620F for 2 hours in a platinum crucible. The melt shall be dissolved in a
limited amount of water, filtered, if necessary, and the solution prepared as in (c).
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