Identification—
A:
Dissolve about 500 mg of ammonium molybdate in 10 mL of sulfuric acid, and add 0.2 mL of Ophthalmic Solution: an intense blue color is produced (distinction from similar amino compounds such as amphetamine and methamphetamine, which, lacking a phenolic hydroxyl, do not undergo this reaction).
D:
Dilute a volume of Ophthalmic Solution, equivalent to about 50 mg of hydroxyamphetamine hydrobromide, with 0.01 N hydrochloric acid to 25 mL, and proceed as directed under
Identification—Organic Nitrogenous Bases 
181
, using
sodium carbonate TS in place of 1 N sodium hydroxide, beginning with “Transfer the liquid to a separator”: the Ophthalmic Solution meets the requirements of the test.
Assay—
Transfer an accurately measured volume of Ophthalmic Solution, equivalent to about 100 mg of hydroxyamphetamine hydrobromide, to a 125-mL separator. Wash the solution with 15 mL of chloroform, and discard the washing. Rinse the stopper and the mouth of the separator with a few drops of water. Add 1.05 g of sodium bicarbonate, preventing it from coming in contact with the mouth of the separator, and swirl until most of the bicarbonate has dissolved. By means of a 1-mL syringe, rapidly inject 0.5 mL of acetic anhydride directly into the contents of the separator. Immediately insert the stopper in the separator, and shake vigorously until the evolution of carbon dioxide has ceased (7 to 10 minutes), releasing the pressure as necessary through the stopcock. Allow to stand for 5 minutes, and extract the solution with five 10-mL portions of chloroform, filtering each extract through a pledget of cotton, previously washed with chloroform, into a tared 100-mL beaker. Evaporate the combined chloroform extracts on a steam bath in a current of air or stream of nitrogen to dryness. Dry the residue at 80
for 90 minutes, cool in a desiccator, and weigh. The weight of the diacetylhydroxyamphetamine so obtained, multiplied by 0.9866, represents the weight of C
9H
13NO·HBr in the volume of Ophthalmic Solution taken.
