Gold recovery from spent materials has been performed on modified cation-exchange resin. The modified resin was prepared by sorption of Rhodamine-B on Dowex-50-X8 (Na+) resin at pH 2.0. Distribution coefficients of gold ion have been determined with 15% (w/v) potassium chloride in different concentrations of hydrochloric acid. On the basis of Kd values quantitative separation of gold from secondary sources has been achieved. Gold(III) has been selectively separated from gold containing spent materials by column chromatography using modified ionexchange resin and the recovery was more than 92% compared to conventional cyanidation process. The results of the proposed method are suggestive of its applicability to other gold containing secondary sources.