Abstract: ⁶³Ni with larger amount of emission and longer half-life in effluent of nuclear power plant should be analyzed, so that the impact of emission from the nuclear power plant on the public can be evaluated accurately. Combined with the enrichment of cationic resin, the separation of nickel specific resin, atomic absorption spectrometer and liquid scintillation spectrometry, a rapid analysis method of ⁶³Ni was established for the effluent of nuclear power plant. Comparison and analysis of liquid effluent samples of nuclear power plant by the establishment method and the national standard GB/T 14502—1993 method, the chemical yield is higher than 70%, the detection limit of this method is 0.005 Bq/L, and the E_n value of the comparison results is far less than 1, indicating that the analysis result of this method is accurate and reliable. In comparison with the national standard method, this method has the advantages of simplicity, fewer steps of separation, higher working efficiency, and is suitable for enrichment and separation of ⁶³Ni in effluent of nuclear power plant.