MIL-DTL-98B
Peak height of H O * p p m M ethanol
p p m H O
2
sample
ISTD
p eak height of M ethanol * Resonse Factor
ppm H2O =
ISTD coulometric KF analysis
2
sample
p p mH 2 O
% H2O =
10,000
DPA Water Analysis Gas Chromatograph Parameters
HP 6890 Series Gas Chromatograph or equivalent
Oven Settings:
Temp
125 deg C
Initial Time
8.00 min
Maximum Temp
250 deg C
Equib Time
0.50 min
Column Parameters
Inlet parameters
8 x ¼" FEP Teflon Porapak PS 50/80 Mesh (or equiv.)
Mode
Splitless
Temp
175 deg C
Pressure
14.7 psi
Flow
233 ml/min
Purge time
75.0
Velocity
1570 cm/sec
Mode
Constant Flow
Gas Type
He
Detector Parameters (Thermal conductivity)
Temp
250 deg C
Ref Flow
25.0 ml/min
Mode
Constant Makeup
Makeup flow
5.0 ml/min
Makeup Gas
He
FIGURE 3. DPA water analysis.
4.2.5 Acidity or alkalinity. Place 20 gm. of an as received sample in a 250 ml.
Erlenmeyer flask and add 50 ml. of nearly boiling distilled water. Stopper immediately and
shake vigorously for about ten minutes. Cool to 25 degrees C. and filter, retaining the
diphenylamine in the flask. Repeat the extraction with 50 ml. of hot water exactly as above. To
the combined filtrates add a few drops of phenolphthalein and titrate with 0.01 normal (N) alkali
if it is acid, 0.01N acid if alkaline. Make a blank titration on the water used and correct the
titration for any acidity or alkalinity found. Calculate the acidity or alkalinity to hydrochloric
acid or sodium hydroxide, respectively. Reserve this solution for the determination of aniline.
4.2.6 Free aniline, aniline salts, and other oxidizable material. Use the solution from the
acid or alkali determination for determining aniline, aniline salts and other oxidizable material by
9
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