Microwave-hydrothermal method was used for synthesis of TiO2 and TiO2 doped with zirconium. Method was fast and simple and adsorbents were used for removal of As(III) and As(V) from aqueous solutions. The adsorbents were characterized by BET surface area measurements and powder XRD. Experiments showed that TiO2 doped with 10% of Zr using microwave-hydrothermal method have greater specific surface area and total pore volume in comparison with TiO2 synthetized with the same method. Better removal with doped adsorbent was obtained for both, As(III) and As(V). Further experiments were carried out with Zr doped TiO2 sorbent in order to examine kinetic of adsorption, influence of pH and effect of common anions present in natural waters.