The new ion exchange resin was synthesized from chloromethylated styrene-1,4-divinylbenzene with crown macrocyclic ligand by substitution reaction. The resin was prepared and the effect of pH, time, dielectric constant of solvent and cross-linked of the matrix on the adsorption for UO₂²⁺, Cu²⁺ and Ho³⁺ was investigated. The metal ion was not adsorbed on the resins pH range below 3 and above pH 4 fast adsorption behavior was showed. The resin selectivity determined in ethanol matrix was in increasing order UO₂²⁺>Cu²⁺>Ho³⁺. In addition, these metal ion was separated on the column packed with 1% crosslinked resin as an eluent.