MIL-DTL-87107E
APPENDIX A
METHOD OF TEST FOR ANALYSIS OF GRADE JP-10 FUEL BY GAS
CHROMATOGRAPHY
A.1
SCOPE
A.1.1 Scope. This method provides for the quantitative determination of the purity of exo-
tetrahydrodicyclopentadiene, the single chemical structure of JP-10. This Appendix is a mandatory part
of the specification. The information contained herein is intended for compliance.
A.2
SUMMARY
A.2.1 Summary of methods. The sample is introduced into a gas chromatograph column, which
has been calibrated with a pure sample of exo- tetrahydrodicyclopentadiene, (4.5). The detector signal is
monitored continuously and the areas of individual peaks are used for computing the quantities of the JP-
10 and other hydrocarbon impurities. The detailed composition of the JP-10 component is computed
from the individual peak areas in the subgroup.
A.3
APPARATUS
A.3.1 Chromatograph. Any conventional gas chromatograph, having at least the following
features, is acceptable.
A.3.1.1 Detector. A thermal conductivity (TCD), flame ionization (FID), or mass spectrometer
(MS) detector may 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, and must be connected to the column in a manner that eliminates cold spots.
A.3.1.2 Temperature Programmer. The instrument must be capable of reproducible
temperature programming over the range of 50⁰C to 300°C. The programming rate must be sufficiently
reproducible so that individual retention times do not vary by more than 2 percent. Any temperature
program, including multilinear modes and intermediate periods of isothermal operation, is acceptable,
provided that the column resolution, as defined in section A.5.2, is not compromised. If capillary-type
columns are used for the analysis, it may not be necessary to program the oven above 200°C.
A.3.1.3 Sample inlet system. Either flash vaporization or on-column injection may be used. For
flash vaporization, the sample inlet port must be maintained between 250° and 300°C, and well-
conditioned septa must be used. If on-column injection is employed, provision must be made for
programming the temperature of the full length of the column. A sample inlet splitter may be used in
conjunction with capillary columns, if care is taken to ensure that a representative sample is delivered to
the column. 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 practice of storing a supply of septa in the
column oven. However, at least one blank run should still be made following each septum change.
A.3.1.4 Column. Either packed or open-tubular (capillary-type) columns may be used, provided
the minimum resolution, specified in A.5.2, is maintained. The column should be designed for maximum
thermal stability and minimum bleed, since the temperature program is likely to run as high as 275°C for
packed columns and 200°C for capillary columns. Dual-column compensation is required if column bleed
results in excessive baseline drift at high temperature.
A.3.1.5 Data Acquisition. Computer controlled data acquisition and integration is the preferred
method of data collection and analysis. The computer system must be designed and calibrated for gas
chromatograph operation. An electric data recorder / integrator may be used if necessary.
A.3.1.6 Microsyringe. A microsyringe, capable of delivering sample volumes from 0.5 to 5.0
microliters, is required for FID and TCD detectors. The widely used 0 10 microliter syringe, Hamilton
Model 701N or its equivalent, is recommended. A microsyringe, capable of delivering sample volumes
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