Abstract: A radiochemical procedure for the separation of ⁹³ Zr based on silica gel separation and TBP extraction was developed. The HLLW solution was first loaded to a silica gel column and was washed with 1 mol/L HNO₃ and then desorbed with 10 mol/L HNO₃.The eluent was extracted with 100%TBP two times. The kerosene was added into the loaded TBP. The ⁹³Zr was stripped with 0.2mol/L HNO₃ twice from TBP-kerosene solution. Subsequently, the 0.2mol/L HNO₃ solution was loaded on the second fresh silica gel column and the separation procedures was repeated. The product ⁹³Zr was measured by HPGe γ spectrometer and liquid scintillation analyzer. The results show the highly effective decontamination of the γ-emitting nuclides. The comparison of liquid scintillation spectra between ⁹³Zr and⁶³Ni indicates that the separated ⁹³Zr sample is radiochemical pure. The whole recovery of ⁹³Zr is about 70%.