Acrylamide/acrylic acid copolymers (AAm/AA) have been synthesized by microemulsion polymerization in absence and presence of trivalent cations Al+3 and Fe+3. Starch materials were obtained by introducing cations Al+3 and Fe+3, in the form of aqueous solutions of sulphates(VI) (modif. starch/Me+3), into the oxidized starch (modif. starch). The flocculation performance of obtained polyacrylamide copolymers and the one based on the natural polymer was compared with the performance of the commercial AAm/AA flocculant (CF). All materials were characterized by capillary viscometry, FTIR and DSC methods. An aqueous suspension of talc was used for the flocculation studies. The flocculation effectiveness was evaluated on the basis of reduction of suspension extinction and the sludge volume. It was found that synthesized AAm/AA/Me+3 copolymers and modif. starch/Me+3 materials exhibit better flocculation properties for a model talc suspension than a commercially available floculant.