MIL-PRF-26536F
APPENDIX A
A.2.2 Gas chromatographic method - capillary column.
A.2.2.1 Procedure. A 30 meters (m) x 0.53 millimeters (mm) DB-Wax, Agilent J & W capillary
column, a TCD, and a split/splitless injector with a glass wool packed split liner shall be used. Table A-1
depicts recommended parameters for initial setup. These parameters may vary depending on GC system
and detector brands, and may be adjusted by the chemist to provide adequate component resolution.
Allow the instrument to stabilize, condition the column and perform check runs by processing three
consecutive injections of 1 - 3 µL of sample. The checks must meet the quality control criteria in A.2.2.2.
This method may be used for aniline quantification for monopropellant hydrazine; for high purity refer to
section E.2.4.
TABLE A-1. GC Recommended parameters
PARAMETER
CONDITION
Carrier Gas
He
Carrier Flow
10 mL/min
Sample Volume.
1 µL (10:1 split)
Inlet Temp.
150 °C
TCD Detector Temp.
200 °C
Carrier + Aux. Flow
~25 mL/min
Carrier + Aux. + Ref. Flow
~65 mL/min
Total (Splitter Bypass) Flow
~90 mL/min
Purge
On
Oven Max
200 °C
Equilibration Time
2.00 min
Initial Temp.(T0)
60 °C
Initial Time (t0)
4.00 min
Rate (1)
10 °C/min
Final Temp. (Tf)
100 °C
Final Time (tf)
0.00 min
Rate (2)
20 °C/min
Final Temp. (2)
185 °C
Final Time (2)
2.75 min
A.2.2.2 Quality control. The following performance criteria must be met for fuel purity analysis,
RSD ≤ 5 %
a
GC replicate analyses (3 consecutive)
a. RSD = Standard Deviation * 100 / Mean
A.2.2.3 Equipment.
(1) Gas chromatograph equipped with a thermal conductivity detector (TCD) and a
split/splitless injector.
(2) Hewlett Packard (HP) Chemstation or equivalent.
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