MIL-PRF-25604F
APPENDIX B
N-NITROSODIMETHYLAMINE
B.1 SCOPE
B.1.1 Scope. This Appendix describes a method for the determination of NDMA, content in the
propellant. This Appendix is a mandatory part of the specification. The information contained herein is
intended for compliance.
B.2 METHOD
B.2.1 Gas chromatographic method.
B.2.1.1 Procedure. A 60 m x 0.53 mm x 1 µm film thickness Stabilwax®-DB megabore column,
a flame ionization detector (FID), a split injector and a deactivated glass wool split liner shall be used. GC
parameters are listed in Table B-1. The analysis requires approximately 14 min for elution of all
components.
TABLE B-1. GC Conditions
PARAMETER
CONDITION
Injector Port Temp.
150°C
Injection Mode
Split injection
Sample Volume
3 µL
Split Ratio
1:50
Carrier Gas
He
Column Flow
10 mL/min
Control Mode
Flow
FID Detector Port Temp.
210 °C
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)
2.75 min
B.2.1.2 Calibration. Prepare a calibration standard equivalent to 100 ppm NDMA by injecting
100 µL of analytical grade NDMA into a 1 L volumetric flask containing approximately 500 mL purified
water. Shake the mixture, dilute to the mark with purified water, and mix the solution thoroughly.
Alternatively, a certified commercially obtained solution may be used and diluted accordingly. If NDMA is
found in the propellant sample, analyze the standard and sample(s) in triplicates; the RSD ≤ 15%.
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