MIL-DTL-11309J
4.5.2.3.1 Calculation. Calculate the result as follows:
Percent surface active ingredient = (mL hyamine)(N hyamine)(M.W.)(dilution)
(10)(sample weight)(aliquot)
Where:
N
=
Normality of hyamine solution (see sections 4.5.1.2.5 and 4.5.1.2.6)
M.W.
=
Molecular weight of LAS (=340)
Dilution
=
Volume of sample (from pouch A) made up to (250 mL)
Aliquot
=
Volume sample solution used for titration (25 mL)
4.5.2.3.2 Preparation of hyamine 1622 (0.002 N). Fill a one-liter volumetric flask half
full with distilled water. Add 0.4 grams 50 percent NaOH slowly and mix. Then add 0.82 grams
of hyamine crystals. Stir until dissolved. Fill to volume with distilled water. For rest of
standardizing procedures, see 4.5.1.2.5.
4.5.2.3.3 Preparation of methylene blue. For preparation of methylene blue, see 4.5.1.2.9.
4.5.2.3.3.1 Reagents.
a. Sodium arsenite (2N) NaAsO2, reagent grade.
b. Sodium hydroxide solution 50 percent, reagent grade.
4.5.2.3.4 Procedure. Wash 32.5 grams of sodium arsenite into a 250-mL volumetric
flask, with distilled water. Add 19.7 mL of 50 percent sodium hydroxide, dilute to volume with
distilled water, and mix well to give 2 N solution. The solution is highly alkaline and susceptible
to air oxidation. It should be stored in a plastic container and dispensed from a dropping bottle.
NOTE: Promptly identify solution with a POISON label.
4.5.2.4 Solubility. Measure one liter of distilled water at 25 șC ± 1 șC into a 1.5-liter
beaker. Weigh out 1 gram of the contents of the pouch A to the nearest milligram. Add carefully
to the distilled water and stir for 2 minutes with a glass rod. Stirring should not be so rapid as to
cause splashing or whipping of the mixture but sufficient to keep the undissolved powder from
settling to the bottom. Withdraw the stirring rod and allow the solution to stand 2 minutes. At the
end of this time, insert a 20-mL pipette about 1 inch below the surface and draw 20 mL into the
pipette. Place the 20-mL sample in a 125-mL Erlenmeyer flask and analyze for titratable chlorine
by the following procedure: Dissolve 1 gram of KI crystals in the 20-mL sample. Add 6 drops of
50 percent acetic acid and swirl to ensure complete mixing. Allow to stand 5 minutes in the dark.
Titrate the free iodine at once with freshly standardized 0.005 N sodium thiosulfate. When the
color is straw yellow, add starch indicator and titrate to end point.
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