Sulphate formed by the oxygen‐flask combustion of foodstuffs may be quantitatively reduced to hydrogen sulphide by a mixture of hydriodic acid, hypophosphorous acid and hydrochloric acid. The gas, swept out by nitrogen, is absorbed in sodium hydroxide solution and titrated with mercuric acetate solution using dithizone as indicator. The difficulties encountered in the method, including interferences, have been investigated and compared with a turbidimetric method. This reduction procedure is recommended where accuracy is required or where elements that interfere with the simpler methods are present.