Abstract: As a growing number of nuclear power units are putting into operation in China, a large amount of radioactive spent ion-exchange resin will be produced. The medium and long half-life radionuclides contained in spent ion-exchange resin are the focus of the safety assessment of disposal site, since they are critical to the long-term safety of disposal site. In this paper extraction chromatography and low background liquid scintillation spectrometry were adopted to establish a method for rapid analysis of ⁹⁰Sr and ⁵⁵Fe in the spent ion-exchange resins of NPP. The results show that the chemical recovery of Sr in this method is 94.94%, and the minimum detectable activity (MDA) is 5.51 Bq/kg, the chemical recovery of Fe using the two separation methods are 96.60% and 87.23%, and the MDA is 10.83 Bq/kg and 11.76 Bq/kg.