Complete mixing of cross-linked phenol-formaldehyde polymeric resin (Duolite XAD-761) with anionic surfactant - sodium dioctyl sulphosuccinate (SDOSS) and EDTA-disodium salt (Chelating agent) in an aqueous solution led to the formation of a modified resin. FT-IR studies showed that the immobilization of the extractants results from hydrophobic interaction between the alkyl group of the extractants and phenyl group of the support, and also from other mechanisms like polar or electrostatic forces. The modified resin was used in batch adsorption experiments for the removal of Ni(II) were carried out as a function of agitation time, pH, adsorbent dosage and adsorption capacity. Adsorption data could be interpretated by Langmuir and Freundlich equations. The results showed that the adsorption kinetics of Ni(II) on modified XAD-761 resin could be best described by the pseudo-second-order model. SEM studies revealed the morphological observations of the pure resin, modified resin and Ni(II) adsorbed modified resin. The adsorbent was also tested for the removal of Ni(II) from synthetic wastewater.