Abstract: Adsorption behavior of Th4+ ions on hydrous sodium titanate (STB) and separation conditions of Pb2+ and Bi3+ on cation- and anion-exchange have been studied in inorganic acid medium of low acidity. Distribution coefficient for Th4 + ions on STB amounts to 106 and quantitative separation of Pb-Bi pair can be obtained. Radiochemical separations of 212Pb from 228Th and 212Bi from 212Pb have been carried out using column experiment. And, from α- and γ-spectra of the eluate samples decontamination factor for 228Th and radionuclidic purity of 212Bi product are determined to be 104 and 97.3%, respectively. The experimental results can be used to prepare 212Pb- 212Bi generator for nuclear medicine therapy.