MIL-PRF-16005F
14.92 ⋅ WC2Na 2O4
=
N KMnO4
VKMnO4
where
N KMnO4
= Normality of potassium permanganate solution
WC2Na 2O4 = Weight of sodium oxalate (g)
VKMnO 4
= Corrected titrated volume of potassium permanganate solution (ml)
4.4.2.2 Assay by densitometer. The procuring activity may accept determination of hydrogen
peroxide assay by density measurement provided a statistical comparison of assay by density versus
assay by titration has been performed and the appropriate conversion tables/equations have been
developed and provided to the procuring activity. The comparison must show that the assay can be
predicted reliably within ± 0.1%. A separate density to assay conversion calculation must be performed
for each type and grade of product. Density measurements must be made within an accuracy of
± 0.00002 g/ml. Any changes to the manufacturing process for each type and grade of product will
require a new statistical comparison of density versus assay by titration.
4.4.3 Sample decomposition. The test methods for anions and ammonium require the
concentrated hydrogen peroxide to be decomposed prior to the analysis. Decompose the sample
utilizing either of the following procedures.
4.4.3.1 Evaporation. Accurately weigh about 40 ml of the hydrogen peroxide sample in a
porcelain or glass evaporation dish. Cover the dish with a ribbed watch glass and decompose the
hydrogen peroxide by carefully evaporating over a steam bath. Rinse the sides of the dish and the watch
glass with reagent water (ASTM D 1193 Type 1) and again evaporate to dryness. Add 10 ml of reagent
water and heat on the steam bath to dissolve the residue. Quantitatively transfer the contents of the dish
to a 50-ml volumetric flask. Rinse the dish and the watch glass at least twice and transfer the washings
to the flask. Dilute to the mark with reagent water and label as decomposed solution. Prepare a blank
solution by treating a 40 ml volume of reagent water in an identical manner.
4.4.3.1.1 Calculation. The concentration of hydrogen peroxide in the decomposed solution shall
be calculated using the following formula:
WH 2O2
=
C H 2O2
V
where
= Concentration of hydrogen peroxide in decomposed solution (g/ml)
C H 2O2
= Weight of sample (g)
WH 2O2
= Volume of decomposed solution (ml)
V
4.4.3.2 Platinum wire catalyzed decomposition in PTFE tubing. This method allows unassisted
decomposition of the concentrated hydrogen peroxide utilizing the apparatus described below.
4.4.3.2.1 Assembly of Apparatus. Obtain a ~20 foot length of 0.125 inch OD, 0.063 inch ID
PTFE tubing. Push a length of 0.032 inch OD stainless steel safety wire through the PTFE tubing. It is
helpful to extend the PTFE tubing out straight. When the end of the stainless steel safety wire comes out
the end of the PTFE tubing, use a cyanoacrylate adhesive (like Super Glue) to attach the end of a 16 foot
length of 0.005 inch OD platinum wire to the safety wire. Allow the glue to set well. Gently pull the safety
wire back through the PTFE tube until the platinum wire is centered in the PTFE tubing. Squirt some
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