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A new heteropolyacid-based cation exchanger zirconium(IV) selenomolybdate has been synthesized, characterized using I.R., X-ray, TGA, DTA techniques. Its composition was found to be Zr:Se:Mo::2.5:0.7:1.6 and it is quite chemically stable. It exhibits 0.94 meq/g ion-exchange capacity for Na⁺ ions. Its distribution behavior for 16 metal ions has been studied and its utility has been employed by achieving separations Zn²⁺–Cd²⁺, Zn²⁺–Co²⁺, Ni²⁺–Cd²⁺and Ni²⁺–Co²⁺ on its column.