MIL-DTL-11751G
that produced by 0.01 milligrams (mg) of chloride ion in an equal volume of solution containing
the quantities of reagents used in the specimen test.
4.5.6 Nitrogen compounds. Dilute 20 mL of solution "A" prepared in 4.5.5 with 50 mL
of ammonia-free water in a flask connected through a spray trap to a condenser, the end of which
dips beneath the surface of 10 mL of 0.1 N hydrochloric acid. Prepare a control by placing 50
mL of ammonia-free water in a similar flask and adding 10 mL of solution "A" and a solution of
an ammonium salt containing 0.01 mg of combined nitrogen. To each flask, add 0.5 g of
aluminum wire in small pieces, allow to stand for 1 hour, and slowly distill about 35 mL. To
each distillate, add 2 mL of freshly boiled 10 percent sodium hydroxide solution, dilute to 50 mL
with ammonia-free water, and add 2 mL of Nessler reagent. Any color produced in the specimen
solution shall be no greater than that produced in the control.
4.5.7 Phosphate.
4.5.7.1 Ammonium molybdate solution. Dissolve 50 g of ammonium molybdate in 1
liter of 1 N sulfuric acid.
4.5.7.2 p-Methylaminophenol sulfate solution. Dissolve 2 g of p-methylaminophenol
sulfate in 100 mL of water. To 10 mL of this solution, add 90 mL of water and 20 g of sodium
bisulfate. Confirm the suitability of the solution by the following test: Add 1 mL of the solution
to each of four solutions containing 25 mL of 0.5 N sulfuric acid and 1 mL of the ammonium
molybdate solution prepared in 4.5.7.1. Add 0.005 mg of phosphate ion to one of the solutions,
0.01 mg to a second, and 0.02 mg to a third. Allow to stand at room temperature for 2 hours.
The three solutions should show readily perceptible differences in blue color corresponding to
the relative amounts of phosphate added. The solution to which 0.005 mg of phosphate was
added should be perceptibly bluer than the blank control.
4.5.7.3 Procedure. To 40 mL of solution "A" prepared in 4.5.5, add 10 mL of
hydrochloric acid and evaporate to dryness on a steam bath. Dissolve the residue in 25 mL of
approximately 0.5 N sulfuric acid, add 1 mL of the ammonium molybdate solution prepared in
4.5.7.1, and 1 mL of the p-methylaminophenol sulfate solution prepared in 4.5.7.2. Allow to
stand for 2 hours at room temperature. Any blue color produced shall be no darker than that
produced by 0.02 mg of phosphate ion in an equal volume of solution containing the quantities
of reagents used in the specimen test, including the residue from evaporation of 5 mL
hydrochloric acid.
4.5.8 Sulfate. Neutralize 250 mL of solution "A" prepared in 4.5.5 with hydrochloric
acid and add an excess of 2 mL of hydrochloric acid. Heat to boiling, add 10 mL of 12 percent
barium chloride solution, digest in a covered beaker on a steam bath for 2 hours, and allow to
stand overnight. If a precipitate is formed, filter, wash thoroughly, and ignite. The weight of the
precipitate shall be no more than 0.0012 g greater than the weight obtained in a complete blank
test.
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