Iron oxide-silica nanocomposites were prepared by sol-gel method using ammonia (NH3), acetic acid (CH3COOH) and hydrochloric acid (HCl) catalysts to generate different pH values for the reaction conditions. As starting precursors, for the silica, respectively, for the iron oxide, tetraethylorthosilicate (TEOS) and iron-III-acetylacetonate were used. The physico-chemical characterization of the materials revealed that the sample obtained with HCl catalyst displays the largest surface area (300m2/g), the most compact network structure, highest surface roughness, biggest crystallite size (14 nm), magnetization (7 emu/g) and superparamagnetic behavior. These materials were tested for adsorption of Cr6+ and Zn2+ from aqueous solution. Sample M-HCl presented the highest surface area and was further used for adsorption of metal ions. Kinetic, thermodynamic and equilibrium adsorption measurements studies were made for Cr6+ and Zn2+. To establish the material behavior from a thermodynamic point of view, temperature and contact time of adsorption process, activation energy, free energy, of standard enthalpy and entropy were calculated. The kinetic behavior was modelled by pseudo-first-order, pseudo-second-order and intraparticle diffusion kinetic models and the adsorption characteristics were determined by modelling the experimental data with Langmuir, Freundlich and Sips isotherms.