Resins with 1-aza-15-crown-5 macrocyclic ligand attached to chloromethylated rene-1,4-divinylbenzene by substitution reaction were prepared and the effect of, metal concentration and cross-linkage of the matrix on the adsorption for UO₂²^+, ²^+ and Sm³^+ was investigated. The metal ion was not adsorbed on the resins pH ○ge below 3 and above pH 4, fast adsorption behavior was showed. The resin ectivity determined in ethanol matrix was in increasing order UO₂²+ $gt; Zn²^+ $gt; Sm³^+. addition, these metal ion could be separated on the column packed with 1% ○sslinked resin by pH 2.5 HNO₃ as an eluent.