Removal of large monovalent cations, as highly toxic thallium (Tl), from the waters is a subject of significant interest due to the hazards its pose. Active materials on the basis of activated carbons intended for removal of Tl ions from drinking water was synthesized and characterized in two stages. During the first, deposition and stabilization of the Fe (3+) phase in the internal surface of activated carbon samples (AC/Fe (3+)) was carry out. During the second, deposition on the AC/Fe (3+) of K4[Fe(CN)6] phase and subsequent chemical reaction were realized. The removal performance of the samples prepared for Tl ions in aqueous solution was investigated by adsorption process. Increased sorption possibilities were observed toward Tl ions as compare to initial carbons.