Abstract: Inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were used together to establish the methods of instrumental analysis and data processing. The activity concentration of ⁶³Ni in the process of preparation of 63Ni β radioactive source from nickel metal after irradiation was measured by the established method in this paper. The measuring results were compared with that from the Liquid scintillation counting (LSC) method. The maximum relative deviation between two methods is 5.1%, and the uncertainty of the measurement results is 4.4% (k=2), which is proved that the method is accurate and feasible.