A procedure for removal and separation of Cs, Eu and activation product of Co using zirconium selenomolybdate was developed. Interactions of134Cs(I),152,154Eu(III), and60Co(II) ions from HNO3acid solutions with zirconium selenomolybdate matrix, dried at 50°C, have been individually investigated by the batch equilibration method. The sorption behavior of the three ions showed a selectivity sequence in the following order: Cs(I) > Eu(III) > Co(II). The breakthrough capacities of zirconium selenomolybdate for Cs(I), Eu(III) and Co(II) were found to be 0.82, 0.45, and 0.18 mmol/g of the sorbent, respectively. A mixture of the three radionuclides (1×10−2 M each) in 140 mL of1×10−2 M HNO3solution was passed through 1 g zirconium selenomolybdate chromatographic column. Thereafter, quantitative elution of the retained Co(II) was achieved with 14 mL of1×10−1 M HNO3acid solution leaving Eu(III) and Cs(I) strongly retained onto the column. Quantitative elution of Eu(III) was achieved by passing 22 mL2.5×10−1 M HNO3. About 89% of the retained Cs(I) was eluted with 32 mL of 2 M NH4Cl solution at a flow rate of 0.5 mL/min.