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| ![]() MIL-P-60335C (MU)
A blank sample of the 1:1 dimethylformamide methanol solution
shall be prepared as described above. A 60 ml. portion of
methanol shall be transferred through the sample porthole Into
the dry titration beaker containing a plastic-coated magnet.
Stopper at once. The magnetic stirrer shall be started and
the water back-titrated in this solvent by adding a slight excess
of Karl Fischer reagent to produce a reddish-brown color which
persists for at least half a minute. The solution shall be
titrated slowly with the water-in-methanol solution until the
exact preliminary end point is reached. All succeeding operations
shall be completed within 3.5 0.25 minutes. 25 ml. of the
supernatant solution shall be rapidly Introduced, accurately
pipetted from the supernatant solution liquid Into the beaker
through the same porthole of the rubber stopper. The porthole
shall be closed immediately and the contents of the beaker stirred
for thirty seconds by means of the magnetic stirrer. A slight
excess (10-15 mls.) of the Karl Fischer reagent shall be added
and carefully back-titrated with the standard water-in-methanol
solution to the final and exact end point. A water determination
of the dimethylformamide-methanol blank solution shall be
conducted as specified above for the extraction of water from
the sample. The percent water in the pyrotechnic sample shall be
calculated as follows:
Calculation:
Percent H20
Std. Blank
Less
Percent Moisture
Leaves
In Sample
Where:
M1s. of Karl Fischer to titrate sample
A
=
Standardization Factor (mg./ml.)
B
=
10
=
Constant Factor
5
=
Standard Sample Weight
4.4.1.3 Alternate method for first fire composition
moisture and illuminant composition moisture.-The moisture content
of the first fire composition and illuminant composition shall
be determined In accordance with Method T101.4, Standard MIL-STD-286.
The temperature setting shall be 100 degrees Centigrade (C) and
the time setting 30 minutes. The sample size shall be between
0.25 and 0,50 grams.
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