Abstract: Anew chelate-forming resin bearing xylenol orange group was prepared by stirring a solution of xylenol orange (XO) with a common anion exchange resin.For the preconcentration of trace heavy metal ions in natural water, the adsorption and desorption behavior of Cu, Zn, Cd, Fe-XOchelates onto an anion exchange resin (Cl-form) by column method was studied, and the atomic absorption spectrophotometric determination of these heavy metals in natural water was established.By this method the recoveries of Cu, Zn, Cd, Fe were 94.3-103, 100-103.6, 90-107, 92-100, respectively, the relative standard deviations for Cu, Zn, Cd, Fe were ±3.4,±2.2, ±1.5, ±0.74% respectively.