Analytical applications of condensed phosphoric acid-III Iodometric determination of sulphur after reduction of sulphate with sodium hypophosphite and either tin metal or potassium iodide in condensed phosphoric acid.

Novel methods for the reduction of sulphate to hydrogen sulphide with hypophosphite-tin metal or hypophosphite-iodide in condensed phosphoric acid (CPA) are proposed. The reduction of sulphate with hypophosphite alone does not proceed quantitatively. Sulphate, however, is quantitatively decomposed with hypophosphite when tin metal or potassium iodide is used together with it. The determination of sulphur by the hypophosphite-tin metal-CPA and tin(II)-CPA methods is interfered with by copper on account of the stabilization of copper(I) sulphide, but this interference can be eliminated by adding iodide, e.g. potassium and lead salts. Alum and barytes are quantitatively decomposed within 15 min at 140 and 280 degrees , respectively. The hydrogen sulphide evolved is absorbed in zinc acetate solution at pH 4.5 and then determined by iodometry.