Diethylenetriamine and a copolymer of sodium acrylate and maleic anhydride were used for the adsorption and separation of Au3+, Ru3+, Bi3+, and Hg2+ ions by forming polymer-metal lolls triple complex. The acidity, temperature, capacity, and interference on the adsorption of these ions on the complex, as well as the conditions of desorption of these ions from the complex, were investigated by means of inductively coupled plasma optical emission spectrometry. The results were satisfactory.