Cerium(III) molybdate nanostructure with average size about 40 nm was prepared by adding cerium(III) chloride and ammonium molybdate solutions under varying conditions. The product was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR), thermogravimetric analysis (TGA) and Brunauere Emmette Teller (BET) techniques. Ion exchange capacity of the sample for potassium ion and distribution coefficients (K-d) for 23 metal ions were determined, the K-d values for TI(I), Pb(II), Th(IV), U(VI), and Cs(I) ions were found to be sufficiently high for their removal from various effluents. The adsorption behavior of the sample towards Cs(I)(134) species were studied. Finally, the binary separation of Dy(III)-U(VI), Sm(III)-Th(IV) and Cs(I)-Rb(I) and removal of Cs(I)(134) from the real sample were successfully achieved. (C) 2012 Elsevier B.V. All rights reserved.