MIL-DTL-45444C
4.7.1.5 Analysis of HMX sample. Reduce the HMX sample
particle size to less than 62 micron. HMX particle size is
usually small enough to permit analysis as received. It may
however, occasionally be necessary to lightly crush the material
in a mortar. Recrystallized HMX requires grinding in a mortar to
reduce the particle size. This is accomplished safely by
grinding 0.1 gram portions in a small mortar. A sample size of
approximately 0.4 gram is required to properly fill the cavity
type sample holder. Press sample into cavity of sample holder.
Place aluminum sample holder (grooved side down) on a very smooth
surface such as polished stainless steel. Place sample into
cavity of holder and press with spatula. Add additional powdered
sample and hand press by placing a stainless steel block over the
cavity area and exerting pressure with hand (50 to 100 lbs is
sufficient). Remove sample and holder and examine surface of
sample on grooved side of sample holder. Sample surface must not
have any voids, cracks, etc. Remove loose explosive from sample
holder. The grooved side of the sample holder must be completely
free of particles prior to insertion into the diffractometer.
Remove shield from diffractometer (shutters must be closed at all
times when intensity measurements are not being made). Insert
sample. The groove on a sample holder must be coincident with
the groove on the goniometer axis of rotation. The rear edge of
the sample holder must be flush against the sample stage.
Replace the shield being careful not to move the sample. If the
electronic panel is maintained ready, move toggle switch to the
up position. Set diffractometer to 16.90 degrees two theta.
Open shutters on X-ray tube tower by pulling out as far as
possible. After 30 seconds, push toggle switch toward scan to
print out time registered on rate meter dekatron tubes. Reset
goniometer to 17.81 degrees two theta. Repeat above. Reset
goniometer to 24.10 degrees two theta. Repeat above. Reset
goniometer to 25.10 degrees two theta. Repeat. Close shutters
on X-ray tower. When no additional samples are ready for
analysis, turn off electronic panel by moving toggle switch
downward.
4.7.1.5.1 Interpretation of data. Record the counts that
are accumulated in 100 seconds, that are printed out under the
respective two theta angle. Place the decimal point two places
to the left in the printout to obtain the representative counts
per second (cps). Subtract cps at 16.90 degree two theta from
cps at 17.81 degrees two theta. This is the intensity (cps) due
to the RDX percent. Opposite the cps obtained, read the RDX
concentration from Fig. 1 (RDX calibration curve). Subtract cps
at 24.10 degrees two theta from the cps at 25.10 degrees two
theta. This intensity is due to alpha HMX. If the RDX
concentration is greater than 1%, determine from Fig. 3 the
correction required by reading the cps opposite the RDX
percentage. Subtract this correction from the cps. From Fig. 2,
read percentage alpha HMX opposite the intensity, (corrected or
uncorrected).
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