Abstract: A method for analyzing 63 Ni in metal has been developed. The metal sample is dissolved with HCl H 2O 2, and the dissolved nickel is separated from other activation products by anion exchange. Nickel is then complexed with pealetyldioxime in the alkaline solution, extracted with toluene, and finally determined by liquid scintillation counter. Chemical yield and Radiochemical yield of this method are 79 3 %±3 2 % and 77 9 %±3 6 %,respectively. Decontamination factor is more than 10 3. The lower detection limit of the method is 20 Bq/g.