MIL-DTL-46225D
yellow disappears, and the solution shall be a very pale blue. Continue titration drop wise with
FP while stirring until the solution turns pink. Divide the volume of CAN by the volume of FP
to get the CAN/FP ratio.
4.6.2.1.3 Standardization of CAN solution. Weigh about 0.3 g of sodium oxalate into a
250 mL beaker. Add a magnetic stir bar. Pipet 40 mL CAN solution into the beaker. Add 25
mL perchloric acid solution. Add two drops ferroin indicator solution. Cover the top of the
beaker with a watch glass, and stir the solution magnetically until all the sodium oxalate is
dissolved. If the yellow color completely disappears, then the aliquot of sodium oxalate was too
large. Try again with a smaller quantity. Titrate the contents of the beaker with FP until the
solution just turns pink.
Normality of CAN N = (100xA)/ {6.701 x (40 BxC)}
Where:
A = weight of sodium oxalate in grams
B = mL of ferrous perchlorate used
C = CAN/FP ratio
4.6.2.1.4 Determination of lead azide purity. Pipet 40 ml of CAN into a 150 mL beaker.
Add 25 mL of perchloric acid solution. Add two drops of ferroin. Cover the beaker with a
watch glass, and place it in an ice bath for fifteen minutes. Use Teflon-coated spatulas and
forceps for handling lead azide. Perform weighings in a high humidity (about 50-60 %)
weighing room. Accurately weigh an amount of approximately 0.4 g of lead azide into a tared
small (1-2 mL) beaker. Using the forceps, plunge the small beaker into the 150 mL beaker.
Wash the forceps tips with a spray of deionized water into the beaker. Gently stir the contents of
the beaker with a glass or plastic stirring rod until all the solid has reacted. If the yellow color
disappears, then the lead azide sample was too large. Repeat with a smaller amount. Titrate the
solution with ferrous perchlorate while stirring until the appearance of a pink color. Calculate the
purity as follows (See 6.11):
Purity of Lead Azide = {14.56 x (40 - BxC) x N}/W
Where:
B = mL of ferrous perchlorate used
C = CAN/FP ratio
N = normality of CAN solution
W = weight of lead azide sample in grams
4.6.2.2 pH. Determine the pH of approximately 1.0 g specimen of lead azide by
suspending in 10 mL of water using a standardized pH meter.
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