USP31--A4专论.doc

Aspirin C9H8O4 180.16 Benzoic acid, 2-(acetyloxy)-. Salicylic acid acetate [50-78-2]. ? Aspirin contains not less than 99.5 percent and not more than 100.5 percent of C9H8O4, calculated on the dried basis. Packaging and storage— Preserve in tight containers. USP Reference standards 11— USP Aspirin RS . Identification— A: Heat it with water for several minutes, cool, and add 1 or 2 drops of ferric chloride TS: a violet-red color is produced. B: Infrared Absorption 197K. Loss on drying 731— Dry it over silica gel for 5 hours: it loses not more than 0.5% of its weight. Readily carbonizable substances 271— Dissolve 500 mg in 5 mL of sulfuric acid TS: the solution has no more color than Matching Fluid Q. Residue on ignition 281: not more than 0.05%. Substances insoluble in sodium carbonate TS— A solution of 500 mg in 10 mL of warm sodium carbonate TS is clear. Chloride 221— Boil 1.5 g with 75 mL of water for 5 minutes, cool, add sufficient water to restore the original volume, and filter. A 25-mL portion of the filtrate shows no more chloride than corresponds to 0.10 mL of 0.020 N hydrochloric acid (0.014%). Sulfate — Dissolve 6.0 g in 37 mL of acetone, and add 3 mL of water. Titrate potentiometrically with 0.02 M lead perchlorate, prepared by dissolving 9.20 g of lead perchlorate in water to make 1000 mL of solution, using a pH meter capable of a minimum reproducibility of ±0.1 mV (see pH 791) and equipped with an electrode system consisting of a lead-specific electrode and a silver–silver chloride reference glass-sleeved electrode containing a solution of tetraethylammonium perchlorate in glacial acetic acid (1 in 44) (see Titrimetry 541): not more than 1.25 mL of 0.02 M lead perchlorate is consumed (0.04%). [note—After use, rinse the lead-specific electrode with water, drain the reference electrode, flush with water, rinse with methanol, and allow to dry.] Heavy metals— Dissolve 2 g in 25 mL of acetone, and add 1 mL of water. Add 1.2 mL of thioacetamide