MIL-PRF-26536F
APPENDIX A
HYDRAZINE ASSAY AND WATER
A.1 SCOPE
A.1.1 Scope. This Appendix describes two Gas Chromatographic methods for the determination
of propellant and water content in the sample. This Appendix is a mandatory part of the specification. The
information contained herein is intended for compliance.
A.2 METHODS
A.2.1 Gas chromatographic method - packed column.
A.2.1.1 Assay column preparation. Cap one end of a 1/8 inch (in) OD by 6 foot (ft) nickel tube
and fill the tube with the Tenax GC column packing by pouring through a small funnel attached to the
other end. Tap or mechanically vibrate the tube to ensure uniform packing. When the tube is filled, plug
both ends with a small wad of glass wool, bend the column to the configuration required by the column
oven, and connect the column to the inlet fitting in the oven. Condition the column with carrier gas flowing
and the oven set at 200°C for one hour. After conditioning the column, connect the other end to the
detector and set the carrier gas flow to approximately 25 milliliters per minute (mL/min), and the column
oven to 50°C. The inlet and detector temperatures, if separately heated, shall be set to 100°C and 150°C,
respectively. The detector current should be set to a nominal sensitivity value recommended for helium by
the instrument manufacturer. The column temperature and carrier gas flow may be adjusted by the
analyst to provide adequate component resolution for minimum analysis time.
A.2.1.2 Procedure. Equilibrate the column with propellant by injection of three or more
1 - 2 microliter (µL) samples into inlet. If more than 30 minutes (min) elapse between analyses, a single
1 µL injection of propellant should re-equilibrate the column. Inject 1 - 2 µL of propellant for analysis and
record the areas of all peaks in the chromatogram, using the following time/temperature program:
Helium carrier gas flow
20 25 mL/min
Initial temperature
50°C
Rate
20°C/min
Final temperature
155°C
Final time hold
4 min
Each analysis should require less than 20 min for elution of all components. The elution order of possible
components is as follows:
Air, ammonia, methylamine, water, and hydrazine.
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