A new mixed metal heteropoly anion-based cation exchanger Zr(IV) molybdo, tungsto vanado silicate (ZMTVS) was prepared under varying conditions. The material was characterized by FTIR, X-ray diffraction, TGA-DTA and SEM techniques. Its ion exchange capacity (IEC) for K+ was found to be 0.86 meq g(-1). Distribution coefficients (K-d) values for 10 metal ions and three radioisotopes were determined. On the basis of Kd values, two important and analytically difficult quantitative binary separations viz. Ni(II)-Co(II) and Ni(II)-Pb(II) were achieved on its column. Decontamination of aqueous nuclear waste solution was also studied. (C) 2009 Elsevier B.V. All rights reserved.