Samples weighing O 2 g are digested with 2 ml of 72 per cent perchloric acid for 2 hr at 180C, and then diluted to 10 ml. with water. After settling, an aliquot of clear solution is reduced with ascorbic-citric acid, and then a zinc dithiol solution is added to form a coloured molybdenum complex which is extracted with petroleum spirit for comparison with standards.Concentrations down to 2 p.p.m. may be analysed at rates up to 150 determinations per day.