Abstract: In order to determine the fission yield and decay γ-ray branch ratio of 127Sb, it is necessary to study the radiochemical separation method of antimony in fission products. In this work, the adsorption performance of Sb(Ⅲ) and Sb(Ⅴ) in hydrochloric acid and nitric acid solutions on five solid phase separation materials was studied, including Dowex 1×4, TEVA, TRU, UTEVA, and silica gel. And the adsorption behavior of the main interference metal ions was discussed in detail. Subsequently, the process conditions of separation related column loading, washing, elution and other operations were optimized. According to the experimental results, a chromatographic separation process using silica gel and TEVA resin was proposed, which was verified using the irradiated uranium target solution. The results show that the chemical yield of antimony in this process is more than 80%, and the decontamination factors of highyield nuclides and main interference nuclides during the measurement of 127Sb γ spectroscopy are all above 1×103. This process is convenient to realize remote automatic operation, avoids valence state adjustment and medium conversion, and does not require the addition of abundant isotope carriers. It is suitable for the radiochemical separation of antimony in the determination of 127Sb fission yield and the preliminary separation in the preparation process of radiochemical pure 127Sb.