MIL-DTL-87173B
APPENDIX C
APPENDIX C
METHOD OF TEST FOR ANALYSIS OF
GRADE PF-1 FUEL BY GAS CHROMATOGRAPHY
C.1 SCOPE
C.1.1 Scope. This method is intended for the analysis of PF-1 Propellant. The method provides for the
quantitative determination of the two major constituents of PF-1 and for the characterization of each
constituent.
C.1.2 Summary of methods. The sample is introduced into a gas chromatographic column. The
detector signal is monitored continuously and the areas of individual peaks are used for computing the
quantities of the methylcyclohexane, exo-tetrahydrodi(cyclopentadiene), and other hydrocarbon
impurities. The detailed composition of the fuel components are computed from the individual peak areas
in the subgroup.
C.2 APPLICABLE DOCUMENTS. (The section is not applicable to this appendix.)
C.3 APPARATUS
C.3.1 Chromatograph. Any conventional gas chromatograph, having at least the following features, is
acceptable.
C.3.1.1 Detector. A flame ionization detector (FID) must be used. The detector shall be operated in
such a manner that its linear dynamic range is not exceeded, and its linearity should be checked
periodically. The detector shall be capable of continuous operation at 300°C or higher, and must be
connected to the column in a manner that eliminates cold spots.
C.3.1.2 Temperature programmer. The instrument must be capable of reproducible temperature
programming over the range of 115° to 250°C. The programming rate must be sufficiently reproducible
that individual retention times do not vary by more than two percent. The temperature program consists
of an initial 12 minutes at 115°C after injection, followed by a programmed temperature rise of 10°C per
minute up to 250°C, and culminating with 10 minutes at 250°C (total run time = 35.5 minutes).
C.3.1.3 Sample inlet system. Flash vaporization shall be used with the sample inlet port maintained at
250°C, and fitted with a well-conditioned septa. A sample inlet splitter set at ~100:1 shall be used in
conjunction with the capillary column described in C.3.1.5.
NOTE 1. New septa should be allowed to condition overnight after being installed in order to minimize
spurious peaks, and several blank runs should be made to purge the column of materials bleeding from
the septum. Overnight conditioning can be eliminated by the expedient of storing a supply of septa in the
column oven. However, at least one blank run should still be made following each septum change.
C.3.1.4 Recorder. Any potentiometric recorder compatible with the chromatograph may be used. The
full-scale response time should be two seconds or less, and the gain and damping controls should be
adjusted to provide optimum response and minimum noise.
C.3.1.5 Column. A 60 meter J&W DB-1 capillary column of 0.25 mm ID and 0.25µ coating, or
equivalent, shall be used.
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