MIL-DTL-14970D
(GC) equipped with a flame ionization detector (FID) and an
electronic integrator. If the electronic integrator is not
capable of printing out a chromatogram a strip chart
recorder shall also be used. The GC shall be fitted with a
1/8 inch O.D. stainless steel column of a suitable length (3
ft or 6 ft may be used) packed with 80-100 mesh Porapak P
(see 6.11) or a 1/8 inch O.D. Teflon lined aluminum column
of suitable length (3 ft or 6 ft may be used) packed with
80-100 mesh Porapak P-S (see 6.9). Prior to performing the
solvent content determination a calibration curve of peak
area versus concentration shall be prepared using
cyclohexanone standards of known concentrations. The
standards shall be made up by appropriate dilutions of a
standard stock solution prepared by accurately weighing 1.0
g to the nearest 0.0001 g into a tared 100 ml volumetric
flask, filling the flask with acetone to the 100 ml mark and
inverting several times to thoroughly mix the solution. The
standard stock solution will contain 0.01 g of cyclohexanone
per ml. Suggested GC conditions are as follows: Carrier
gas pressure 50 psig (suggested for a
3 ft or 6 ft column); injection temperature 135 to 150oC,
oven temperature 190 to 210oC; detector and outlet manifold
temperature 200 to 210oC; recorder (if used) chart speed
0.5 cm/min and injection volume 1.0 microliters.
Appropriate calibration solutions shall first be injected
and their peak areas determined. The calibration curve
shall be constructed. An approximate 5.0 g sample of
Composition A-5 shall be weighed to the nearest 0.0001 g and
transferred to a 100 ml volumetric flask and acetone shall
be added to below the 100 ml mark in order to dissolve the
sample. After the sample has dissolved acetone shall be
added to the 100 ml mark and the flask inverted several
times to thoroughly mix the solution. A 1.0 microliter
portion of the sample shall be injected into the GC. The
percent of cyclohexanone solvent shall be calculated using
the following equation:
Cyclohexanone solvent, percent = 100 (A x C)
BxS
Where:
A
=
the cyclohexanone peak area in integrator
units(IU) of the sample
B
=
the average peak area in IU of the standard
sample injection having a peak area nearest
to the sample peak area
C
=
the concentration in g/ml of cyclohexanone in
the standard sample as above and
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