MIL-DTL-46225D
optical microscope using magnifications of 50x to 200x, using a systematic approach to view a
significant portion of the particles. At least 1 photomicrograph of each sample shall be retained.
Particles shall be similar to those in Figures 1, 2, or 3. Particles as shown in Figure 4 or 5 are
unacceptable and the batches of lead azide containing such particles shall be rejected.
4.6.2 Chemical tests.
4.6.2.1 Purity. (see 6.8.2 for precaution)
4.6.2.1.1 Solutions for purity determination.
a. Ceric Ammonium Nitrate (CAN). Dilute with deionized or distilled water 60
mL of 70-72 % perchloric acid solution to approximately 700 mL, and add this
solution to 60 g of reagent grade ceric ammonium nitrate. Heat and stir the
mixture until solution takes place. Depending on the source CAN solutions can
appear perfectly clear or have considerable insoluble matter. Allow to cool and
let stand for forty eight hours. Filter the solution through a Gooch crucible fitted
with GF/F filter mats to eliminate all insoluble matter.
b. Perchloric acid solution. Dilute with deionized or distilled water 60 mL of 70-
72 % perchloric acid solution to a volume of 1 liter.
c. Ferrous Perchlorate solution (FP). This may be prepared in two ways.
1. Commercially available ferrous perchlorate can be used, if the color is still
green. A brown color indicates the iron has oxidized to ferric and is no longer
usable. Add 30 g of the solid ferrous perchlorate into a liter beaker. Add 700
mL deionized or distilled water and 60 mL of 70-72 % perchloric acid. Stir
until all solid is dissolved. Filter through a Gooch crucible fitted with GF/F
filter mats and make the volume up to 1 liter. Pass nitrogen gas through the
solution for two hours before using. Store solution in a closed container.
2. The second method involves making the solution from iron wire and
perchloric acid. Add 6 g of iron wire into a liter beaker. Add 700 mL
deionized or distilled water and 60 mL of 70-72 % perchloric acid solution.
Heat beaker on a steam bath in a fume hood until the metal dissolves. There
will be black residue. Filter through a Gooch crucible fitted with GF/F filter
mats. Make volume up to 1 liter. Pass nitrogen gas through the solution for
two hours before using.
d. Ferroin indicator solution. Commercially available ferroin indicator can be
used.
4.6.2.1.2 Determination of CAN/FP ratio. Pipet 40 mL of the CAN solution into a 150
mL beaker. Add 25 mL of perchloric acid solution. Add two drops of the ferroin indicator
solution. The color shall be yellow. Titrate with FP. Gradually the color lightens until the
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