MIL-PRF-27404D
APPENDIX A
MONOMETHYLHYDRAZINE 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) outer diameter (OD) by 6 foot
(ft) nickel tube and fill the tube with the Tenax®-TA 60/80 mesh 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 helium 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 100°C. The inlet and detector
temperatures, if separately heated, shall be set to 150°C and 210°C, respectively. The detector current
should be set to a nominal sensitivity value recommended for helium by the instrument manufacturer.
A.2.1.2 Procedure. Equilibrate the column with propellant by injection of three or more
1 microliter (μL) samples into the inlet. If more than 30 minutes elapse between analyses, a single
1 μL injection of propellant should re-equilibrate the column. Inject 1 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
45 mL/min
Initial temperature
100 °C
Initial time
2 min
Rate
20 °C/min
Final temperature
200 °C
Final time
3 min
Each analysis should require less than 15 minutes for elution of all components. Hydrazine elutes at the
leading edge of the MMH peak. If observed, traces of hydrazine shall be included in the reporting of
MMH.
The elution order of possible sample components is as follows:
Air < ammonia < water < methylamine < hydrazine < MMH.
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A.2.1.3 Calculations.
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