Abstract: In order to improve the accuracy of the fission yields of ¹⁵⁶Eu and ¹⁶¹Tb in neutron-induced uranium fission, radiochemical purity sample of ¹⁵⁶Eu and ¹⁶¹Tb has to be obtained. A separation procedure of Eu and Tb from uranium, aluminum and fission products was established in this paper. Aluminum was first removed by hydroxide co-precipitation method, then uranium was removed by calcium fluoride co-precipitation method, and rare earth elements were recovered by 30% TRPO-kerosene extraction method, Eu and Tb were separated from the mixed rare earth elements by cation exchange chromatography method. When the sample contains 2 g uranium, 0.65 g aluminum and fission products, the chemical recoveries of Eu and Tb are better than 80%, the decontamination factors are greater than 106 for U, ²³⁹Np, ⁹⁵Zr, ¹⁰³Ru, ¹³¹I, ¹³²Te, ¹⁴⁰Ba, ¹⁴⁰La, ¹⁴¹Ce and ¹⁴⁷Nd. The method can meet the requirement of measurement of ¹⁵⁶Eu and ¹⁶¹Tb yield in neutron-induced uranium fission.