MIL-DTL-45444C
4.7.1.1.2 Preparation of alpha HMX calibration standard.
Add 4 grams of the purified beta HMX to 80 ml of (70% by weight)
nitric acid. Heat until the HMX dissolves. Filter the solution
with filter paper and cool slowly to 30 degrees C. After one
hour, filter the slurry using a medium porosity crucible. Wash
the precipitate thoroughly with distilled water. Dry in a vacuum
oven at 60 degrees C for two hours. Alpha morphology shall be
verified by microscopy or infrared spectroscopy before the alpha
HMX is used as a calibration standard.
4.7.1.2 Purity analysis of RDX standard. Prepare RDX
solvent by stirring 1,2 dichloroethane at room temperature for
four hours in contact with HMX crystals. Solubility of HMX in
1,2 dichloroethane at room temperature (24 degrees C) is 0.02
gram per 100 ml. Accurately weigh approximately 0.2 gram of the
RDX calibration standard to the nearest 0.1 milligram into a
tared 125 ml glass stoppered conical flask. Add 100 ml of 1.2
dichloroethane that has been saturated with HMX. Secure the
glass stopper and shake the flask on a wrist action shaker for
one hour. Accurately weigh a fine porosity 30 ml fritted glass
crucible and place it on a filtering flask. Apply vacuum to the
filtering flask and transfer the sample residue from the conical
flask to the crucible. Rinse the contents of conical flask into
the crucible with saturated 1,2 dichlorethane. Wash residue in
the crucible 2 times with 100 ml portions of diethylether. Suck
dry under vacuum for 15 minutes. Allow the crucible to come to
room temperature and weigh crucible and insoluble residue. The
insoluble residue is HMX. Therefore, the percentage of RDX in
the sample is:
(A-B) x 100
A
Where:
A - is the original sample weight in grams.
B - is the insoluble residue weight in grams.
4.7.1.3 Preparation of calibration standard samples.
Prepare 5 gram samples of the calibration standard mixtures
listed in Table IV as follows: Accurately weigh to the nearest
0.1 milligram the ingredients listed in Table IV (use purified
materials which pass through a US Standard Sieve No. 260) in the
proper proportions to yield a 5.0 gram sample. Place the
ingredients in 250 ml Erlenmeyer flasks and mix thoroughly for a
minimum of three hours with the aid of a wrist action shaker.
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