Tin(IV) antimonate (SnSb), cerium(IV) antimonate (CeSb), silicon(IV) antimonate(SiSb) ant titanium(IV) antimonate (TiSb) were prepared under various conditions. The ion-exchange properties and the thermal stability of these materials were examined in order to elucidate their applicability to the processing of radioactive liquid wastes. Capacity, equilibrium measurements, adsorption isotherms and the selectivity patterns for Cs+, Sr2+, Co2+ and Eu3+ ions on these sorbents at different conditions were determined. The effect of high concentrations of salts and complexing agent as interfering ions in the feed solutions on the distribution coefficient of the metals, mentioned above, was tested as a function of [HNO3]. Based on the results obtained, practical separation experiments on column were performed.