Abstract: ICP-AES was applied to the determination of vanadium in ammonium metavanadate. The sample was dissolved with 50 g·L-1 oxalic acid solution, and the spectral line of 310.230 nm was selected as analytical spectral lines for V. Linear relationship between values of spectral line intensity and mass concentration of V was kept in the range within 50 mg· L-1, with detection limit (3S/N) of 0.02 mg·g-1. The proposed method was used in the analysis of two ammonium metavanadate samples, the results obtained by the present method were a little higher than those obtained by titrimetry. Values of recovery found by standard addition method were in the range of 99.8%-101.8%, with values of RSD (n=5) less than 0.3%.