Silicotitanate, molybdotitanate, and chromotitanate as inorganic ion exchange materials were synthesized with Si/Ti, Mo/Ti, and Cr/Ti ratios equal to 1.0, 1.33, and 0.5, respectively. The chemical composition of the synthesized materials were determined and found to SiTiO4 center dot 9.52H2O, Mo4Ti3O16 center dot 10.2H(2)O, and Cr2Ti4O11 center dot 5.65H(2)O for silicotitanate, molybdotitanate, and chromotitanate, respectively. Schematic illustrations of these materials were achieved according to the related structures. The stability of these synthesized materials in different media showed high resistance toward chemical attack. Batch adsorption technique was used for the investigation of the distribution coefficients of Cs-134, Co-60, and Eu-152,Eu-154 from synthetic mixture solutions on the three inorganic ion exchangers. The effect of the medium composition (pH) on the distribution coefficients was studied, and the data obtained indicated that 6 Co had a very low distribution coefficient on the three ion exchangers in 0.1 M HNO3 and a mixed system of 0.1 M HNO3 + 0.1 M NaNO3. 134Cs and Eu-152.154 are highly adsorbed on molybdotitanate and chromotitanate in 0.1 M HNO3 medium; on the other hand, these ions have high distribution coefficients on silicotitanate in 0.1 M HNO3 + 0.1 M NaNO3 medium. Based on the batch distribution coefficient data achieved, chromatographic column separations of Cs-134-(60) Co, Cs-134-Eu-152,Eu-154, and Co-60-Eu-152,Eu-154 were carried out using different eluants such as 0.01 M HNO3, 0.1 M HNO3, 0.1 M NH4Cl, and 0.1 M NH4OH.