Resins with 1-aza-15-crown-5 macrocyclic ligand attached to chloromethylated irene-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⁺, Zn²⁺, and Sm³⁺ was investigated. The metal ion was not adsorbed on the resins pH age below 3 and above pH 4, fast adsorption behavior was showed. The resin selectivity determined in ethanol matrix was in increasing order UO₂²⁺ > Zn²⁺ > Sm³⁺. addition, these metal ion could be separated on the column Packed with 1% crosslinked resin by pH 2.5 HNO₃ as an eluent.