MIL-PRF-87930B
APPENDIX A
HYDRAZINE ASSAY AND WATER
A.1 SCOPE
A.1.1 Scope. This Appendix describes a Gas Chromatographic method for the determination of
hydrazine 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 METHOD
A.2.1 Gas chromatographic method capillary column.
A.2.1.1 Procedure. A 60 meter (m) x 0.53 millimeters (mm), 1.00 micrometer (µm) film thickness
Agilent DB-Wax capillary column, a TCD, with a split injector and a glass wool packed split liner shall be
used. Table A-1 provides a summary of the critical operating parameters. These parameters may vary
depending on GC system, detector brands, and column length and may be adjusted to optimize
component resolution.
TABLE A-1. GC and method parameters
CONDITION
PARAMETER
Injector Port Temp.
150 °C
Injection Mode
Split injection
Sample Volume
1 µL
Split Ratio
1:50
Carrier Gas
He
Control Flow
10 mL/min
Control Mode
Flow
TCD Detector Temp.
210 °C
Equilibration Time
2.00 min
Initial Temp.(T0)
60 °C
Initial Time (t0)
3.00 min
Rate (1)
10 °C/min
Final Temp. (Tf1)
100 °C
Final Time (tf1)
0.00 min
Rate (2)
20 °C/min
Final Temp. (Tf2)
185 °C
Final Time (tf2)
3.75 min
The elution order of possible sample components is as follows:
Air > ammonia > water > hydrazine > aniline
A.2.1.2 Standard preparation.
Determine the hydrazine and water content of a sample of high purity hydrazine (HPH) using
procedures in the latest revision of MIL-PRF-26536. Use this analyzed hydrazine to prepare a mixture
with purified water which is approximately 70% hydrazine and 30% water. Use an analytical balance that
is accurate to 0.1 mg to determine the weight of each component used to make the standard. (Use
approximately 0.5 mL H2O for each 1 mL of N2H4).
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