Samples weighing 05 g are fused with sodium hydrogen sulphate, leached with 5 ml. of 4 M nitric acid and diluted to 10 ml. with water. An aliquot of the clear solution is boiled with concentrated nitric acid and then 2 ml. of a phosphotungstate solution are added. After dilution to 10 ml. with water, the solution is heated in a boiling water-bath for not less than 10 min. When cold, the solution is extracted with 2 ml. of iso-amyl alcohol and the yellow phosphotungstovanadate complex is compared with a standard series. Concentrations down to 4 p.p.m. may be analysed at a rate of 100 samples per man-day of 8 hr.