MIL-PRF-16005F
samples. Flasks that give inconsistent results shall be rejected. Flasks that give consistent results shall
only be used for hydrogen peroxide samples.
4.4.6.4 Reagents and equipment.
a. Reagents:
Nitric acid: Concentrated, ACS reagent grade.
b. Equipment:
(1) Flask: Volumetric, pyrex, 50-ml, 3 required with 4-inch extension on flask neck.
(2) Aluminum: Foil, pure.
(3) Balance: Analytical, 0.1 mg sensitivity.
(4) Water or steam bath.
(5) Beaker: Glass, small, 3 required.
4.4.7 Evaporation residue.
4.4.7.1 Procedure. Add several pieces of clean platinum that have a surface area equivalent to
the inside of two 100-ml casseroles into a clean 2-liter pyrex beaker containing 500 ml of reagent water
(ASTM D 1193 Type 1). Cover the beaker with a clean, ribbed watch glass and place it on a hot plate.
Add 300 ml of the sample in not larger than 50-ml increments. Between increments, allow the major
portion of each increment to decompose. If the solution is maintained at boiling, decomposition of the
total solution will require 2 to 4 hours. Immediately prior to total decomposition, transfer the solution to a
clean 1-liter Pyrex boiling flask and cover it with a clean ribbed watch glass. Add a small piece of clean
platinum to the solution to prevent concentration of any remaining hydrogen peroxide in the sample. Boil
the solution until condensed to a 25 to 50-ml volume. Transfer the remaining solution to a 100-ml
platinum evaporating dish that has attained constant weight by heating. Allow the solution to completely
evaporate. While decomposing and condensing the sample, add 500 ml of reagent water to a clean 1-
liter Pyrex boiling flask and cover it with a clean ribbed watch glass. Place the flask on a hot plate and
boil until condensed to a 25 to 50-ml volume. Discontinue boiling and transfer the remaining water to a
100-ml platinum dish that has attained constant weight by heating. Place the dishes in a vacuum oven at
105° to 110°C (221° -230°F) for a minimum of 1 hour. Remove the dishes and allow them to cool in a
desiccator. Place on a balance and record the weight to the nearest 0.1 milligram.
4.4.7.2 Calculation. The evaporation residue of the sample shall be calculated as follows:
WR
ER =
0.3
where
ER = residue in mg L
WR = corrected weight of residue in mg
4.4.7.3 Reagents and equipment.
a. Reagents:
Water: ASTM D 1193 Type 1
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