Abstract : An accurate method is proposed for the determination of zirconium in zirconium metal and zirconium powder. The sample is dissolved in a mixture of hydrofluoric, nitric, perchloric, and sulfuric acids, the solution is evaporated to dryness, the salts are dissolved in dilute hydrochloric acid, mandelic acid is added, the solution is heated at 80 deg C. for 40 minutes, the zirconium mandelate is filtered off, the residual zirconium in the filtrate is recovered by heating at 80 deg C. overnight, and the combined precipitates are ignited over a blast burner to zirconium dioxide. An investigation was made of the factors involved in the dissolution of the sample, precipitation with mandelic acid, ignition of the precipitate, and size of the sample. The effect of hafnium and possible interferences was considered.