Abstract: A simple and rapid method for the determination of sodium stibogluconate is proposed and the procedure is summarized below: Dissolve about 0.2 g of sodium stibogluconate,accurately,weighed,in 50 ml of water,and add to it 50 ml of 3 N hydrochloric acid and 2.5 g of potassium iodide.Keep this solution in a dark place for 30 minutes.Titrate the liberated iodine with 0.1 N solution of sodium thiosulfate,using starch solution as indicator. 1 ml of sodium thiosulfate is equivalent to 6.088 mg of Sb. The tri-valent antimony formed by the reaction in the solution reacts with the excess potassium iodide added and produces a light yellow coloration,owing to the formation of a complex salt,but it does not interfere with the end point. This method is compared with that of Chinese Pharmacopoeia 1953,British Pharmaceutical Codex 1949,New and Non-official Remedies 1950,and a modified method of that described in the British Pharmaceutical Codex 1949,showing favourable results.