This study deals with the synthesis of stannic silicomolybdate (SnSiMo) using the sol-gel technique, and used for the first time in a separation of Y(III) from Zr(IV)-Y(III) as a simulation mode for the purification of Y from its daughter (Zr). The produced material was physically characterized by XRF, FTIR, XRD, TGA, and SEM. Its composition was found to be [(SnO2)(3). (H2SiO3). (H2MoO4)(3)]. 6H(2)O. The prepared SnSiMo possesses high chemical and thermal stabilities. The sorption behaviors of yttrium and zirconium on the prepared ion exchanger were studied as a function of pH. It was found that SnSiMo had the highest distribution coefficient (K-d) for Y(III) as compared to Zr(IV). Using a column packed with SnSiMo, Y(III) was separated from Zr(IV)-Y(III) using 0.1, 0.2, 0.5, and 1 M HNO3. The separation of Y(III) from Zr(IV)-Y(III) group was achieved successfully.