MIL-DTL-398D
c. The crucible shall be aspirated during the transfer
process and the crucible and contents shall be aspirated for
approximately 2 minutes after the transfer has been completed.
The suction shall be turned off and 15 ml. of anhydrous methanol
added to the crucible and contents; the methanol shall be allowed
to remain in contact with the explosive for approximately 5
seconds and then removed with the aid of suction. The contents
of the crucible shall be washed once more with anhydrous methanol
as described above and then the crucible and contents shall be
aspirated until the odor of methanol is no longer discernible.
The crucible and contents shall be dried in an oven maintained at
105 degrees C plus or minus 2 degrees for 15 minutes or
equivalent method, cooled in a desiccator and weighed.
d. The weight of material retained on each sieve shall be
determined and the percentage passing through each sieve
calculated on the basis of the dry weight of the RDX sample to
determine compliance with 3.3 and Table II.
4.7.7 Analytical method for RDX purity and HMX content. A
high performance liquid chromatographic (HPLC) method will be
used to determine RDX purity by quantifying the concentration of
HMX impurity in the RDX product.
4.7.7.1 HPLC method conditions. The HPLC system used in the
analysis of RDX product and appropriate method calibration
standards shall be comprised of a column, mobile phase, pumping
system, sample injection system, detector system and data capture
system. The column used in the testing shall be a MicroBondapak
CN (10 micron particle size, 3.9 mm x 150 mm Internal Dimensions
(see 6.6) or a direct column equivalent. The mobile phase shall
be a quaternary system consisting of the following components and
volumetric proportions: 70% by volume, 2,2,4-trimethylpentane
(iso-octane), 15% by volume of acetonitrile, 7.5% by volume
chloroform, and 7.5% by volume of methanol. All solvents used in
the mobile phase shall be vendor certified as HPLC grade
chemicals. Prior to use in the testing, the mobile phase should
be thoroughly degassed using either vacuum degassing techniques
or by purging with an inert gas. The injector component within
the HPLC system shall be equipped with a sample loop capable of
delivering a 20 microliter injection volume of sample to the HPLC
column. The detection system used in this HPLC testing shall
utilize an ultraviolet (UV) detector having a light wavelength of
254 nanometers.
4.7.7.2 HMX (beta) and RDX calibration standards. High
purity HMX (beta) and high purity RDX suitable to be used as
calibration standards are available from several sources.
(See 6.11).
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