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Page Title:
Determination of normal lead styphnate (when applicable) |
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|  MIL-D-70603(AR)
with the residue for approximately 2 minutes. The residue shall be
washed with water until the filtrate coming through the crucible
appears colorless. The filtrate and washings shall be
quantitatively transferred to a 250 ml. calibrated volumetric flask,
the beaker washed thoroughly with distilled water and diluted to the
mark. Using a calibrated pipette, a 2 ml. aliquot of this solution
shall be transferred to a 50 ml. calibrated volumetric flask and
diluted to the mark with distilled water. A portion of this section
shall be transferred to a corex glass spectophotometric cell (see
6.4)having a width of approximately 1 centimeter (cm.) and its
absorbance density determined at a wave length of 410 millimicrons.
As reference, a similar cell containing acetate solution of the same
concentration as the sample solution shall be used. Since the cell
which holds the basic lead styphnate is not identical with the
reference cell, the absorbance density obtained shall be corrected
as described above for the difference in the amount of light which
the two cells scatter and absorb. To do this, both cells shall be
filled with ammonium acetate solution and the absorbance density of
the cell which originally contained the basic lead styphnate
solution shall be measured at a wave length of 410 millimicrons.
The percentage of basic lead styphnate in the sample shall be
calculated on a dry basis as follows:
F(A-B)
Basic lead styphnate, percent =
w 1-.O1M) D
Where:
A = optical density of basic lead styphnate solution
B = optical density of ammonium acetate solution
D = width of
cm.
corex cell,
M = moisture content of sample obtained from 4.3.3 in
percent
w = weight of sample
factor to be determined for each instrument on the
F=
basis of a sample of lead styphnate that is suitable for use as a
standard.
4.5.4.3 Determination of normal lead styphnate (when
applicable). Extract the residue obtained in the barium nitrate
determination with sufficient 5 ml. portions of ammonium acetate
solution (saturated) at about 25 until the washings are
colorless. Agitate each portion for about 1 minute, then allow each
portion to remain in contact with the residue for one additional
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