MIL-PRF-16005F
4.2.2.1.4 Tanks. Samples shall be taken by means of a sampling thief or other accepted device
from each portable tank, cargo tank, or tank car. One sample shall be drawn within one foot of the
surface, one near the midpoint, and one within one foot of the bottom.
4.3 Rejection. When any sample of the propellant tested in accordance with 4.2 fails to conform
to the requirements specified herein, the entire lot represented by the sample shall be rejected.
4.4 Test methods.
4.4.1 Examination of Product. One twenty-five milliliter (ml) specimen shall be taken from each
of the samples and shall be placed in separate laboratory glass test tubes. Each separate test tube shall
be visually inspected across the diameter of the tube and compared with a similar tube of reagent water
(ASTM D 1193 Type 1) to verify conformance with this specification as to clarity and color. (see 3.4).
4.4.2 Hydrogen peroxide assay. Hydrogen peroxide assay shall be determined by one of the
following procedures. In the event of dispute, the procedure specified in paragraph 4.4.2.1 shall be the
referee method.
4.4.2.1 Assay by titration.
4.4.2.1.1 Procedure. Accurately weigh about 1 ml of sample in a tared 100ml volumetric flask,
dilute to volume with reagent water (ASTM D 1193 Type 1) and mix thoroughly. Transfer exactly 20.0 ml
of this solution to a 250 ml conical flask, add 20 ml of 2.5N H2SO4 solution and titrate with standardized
0.5 N (0.1M) potassium permanganate to a pink color that persists for 15 seconds. Correct the volume
by titrating a blank aliquot to the same endpoint. The titrant shall be at the same temperature during the
assay and the standardization.
4.4.2.1.2 Calculation. The percent H2O2 by weight shall be calculated by the following formula:
8.5 ⋅ V
⋅N
KMnO 4
KMnO 4
=
%H 2 O 2
W
H2O2
where
V
= corrected volume(ml) of potassium permanganate
KMnO 4
N
= normality of potassium permanganate
KMnO 4
W
= weight of sample (g)
H 2O2
4.4.2.1.3 Standardization of potassium permanganate solution. Bring 500 ml of dilute sulfuric
acid (one volume concentrated acid plus 19 volumes of reagent water) to a boil and allow to cool.
Separate into two 250ml aliquots. Dissolve about 1.50 g, weighed to the nearest 0.1 mg, of reagent
grade sodium oxalate (dried at 105°C) into one of the aliquots and save the other aliquot as a blank.
From a burette, add 39 - 40 ml of the potassium permanganate solution to the oxalate solution at a rate of
25 35 ml per minute while stirring slowly. Allow the solution to stand until the pink color has
disappeared, then heat to 55-60°C and continue the titration, while stirring slowly, until a faint pink color
(sighted on a white background) persists for 30 seconds. Correct the volume by titrating the blank acid
aliquot to the same endpoint. Calculate the normality of the potassium permanganate solution as follows:
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