Abstract: A simplified volumetric method for the determination of sulfur in organic compounds is described. The results obtained by this method are in agreement with those obtained by the gravimetric method, The method is stated as following: Weigh accurately a sample containing 30—75 mg SO₄^- into a nickel crucible containing 1 g. of KNO₃ and 8 g. of KOH. Heat the crucible carefully with a small flame until the contents melt, increase the heat gradually until the decomposition is complete. Leach the melt with water, acidify with HCl and heat gently until bubbles cease to evolve. Filter, dilute the filtrate to about 60 ml. and after neutralizing with 6N NH₄OH, add 0.2 ml. 6N HCl. Heat to 70℃, add gradually the benzidine hydrochloride reagent to precipitate the sulfate in the solution. After cooling in an ice bath for 1 hour, the precipitate is filtered from the solution. Suspend the precipitate in water, heat to 80℃ and titrate with 0.1N NaOH solution, using phenolphthalein as indicator.