Abstract:A method for the determination of nickel in cobalt powder by atomic absorption spectrometry after extraction separation was studied. In ammonia medium at pH 8-9, the dimethylglyoximenickel complex was extracted by chloroform using citric acid as stabilizer. After reextraction with hydrochloric acid, the content of nickel in reextraction solution was determined by atomic absorption spectrometry. The matrix and coexisting elements after extraction separation had no interference in the determination of nickel. The detection limit of method was 0.002 % (mass fraction). The absorbance was linear to the mass concentration of nickel in range of 0.4-150 μg/mL with correlation coefficient higher than 0.9996. The method was applied to the determination of micro nickel in cobalt powder. The results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICPAES). The relative standard deviation (RSD, n=11) was less than 2.7 %.