This paper presents the results of the preparation of di(2-ethylhexyl)phosphoric acid (D EHPA)-impregnated Amberlite 2 200 resin and its application for the separation of Ni, V and Mo ions in sulfuric acid solution. The advantages of choosing this system are mainly due to the distinct metal ions extraction behavior of D EHPA and Amberlite 200 resin. At low pH 2 value, Amberlite 200 can sorb much higher amounts of Ni ion than V and Mo ions. D EHPA can extract higher amounts of 2 Mo ion than V and Ni ions at low pH value. The impregnation of D EHPA into Amberlite 200 modifies the metal ion 2 sorption behavior of the resin. Three impregnation procedures were proposed to prepare the D EHPA-impregnated resin. 2 Surface modification with sodium dodecyl sulfate surfactant converts the hydrophilic surface of Amberlite 200 into hydrophobic nature, which improves the impregnation of D EHPA. The highest amount of impregnated D EHPA was about 2 2 0.26 g in 1.0 g of dry Amberlite 200 resin. In order to realize the effects of operation parameters on impregnation process, the characteristic properties of Amberlite 200 were investigated using the Brunauer-Emmett-Teller (BET) method and ESCA (electron spectroscopy for chemical analysis) to interpret the possible mechanism of impregnation. The sorption of Ni ion on D EHPA-impregnated resin reduces to 33% of that on non-modified resin. The sorptions of Mo and V ions, however, 2 increase by about nine and four times compared to those on non-modified resin, respectively. The results of selective extraction of mixed ion solution further demonstrate the feasibility of using D EHPA-impregnated Amberlite 200 resin for 2 the separation of mixed Ni, V and Mo ions.