Spent pickling liquors from leaching copper ore concs. with 10% NH4OAc were treated with 3 ion-exchange resins under lab. conditions (column diam. 0.65 cm, column height 60 cm, wastewater flow rate 2 cm(3)/min) and analyzed for Cu and Pb with automatic spectrum analyzer. The degree of the ion removal was 77-96% for Cu and 71-99% for Pb. The highest efficiency showed the resin with amino groups.