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Method of Assay
Accurately weigh about 0.5 g of the sample and dissolve in a 10% sulfuric acid solution and dilute to 100 ml with the same acid. Introduce 5.0 ml of this solution into a long-necked combustion flask, add 10 ml of sulfuric acid TS and heat gently until gas is no longer evolved. Boil gently for 10 min, cool and add cautiously 40 ml of water. Cool again and place in a steam-distillation apparatus. Add 50 ml of 10 N sodium hydroxide solution and distill immediately by passing steam through the mixture. Distil for 1 hour, collecting about 50 ml of distillate in 40 ml of a 4% w/v solution of boric acid. Add 0.25 ml of methyl red/methylene blue TS and titrate with 0.1 N hydrochloric acid. Carry out a blank determination. Each ml of 0.1 N hydrochloric acid is equivalent to 3.003 mg of CH4N2O.
Steven