The presence of arsenate in drinking water causes adverse health effects including skin lesions, diabetes, cancer, damage to the nervous system, and cardiovascular diseases. Therefore, the removal of As (V) from water is necessary. In this work, nanostructured adsorbent Fe2O3/Al2O3 was synthesized via the sol-gel method and applied to remove arsenate from polluted waters. First, the Fe2O3 load of the adsorbent was optimized. The Fe2O3/Al2O3 adsorbent was characterized by means of XRF, XRD, ASAP, and SEM techniques. The effects of the operating conditions of the batch process of As (V) adsorption such as pH, adsorbent dose, contact time, and initial concentration of As (V) solution were studied, and optimized. The thermodynamic study of the process showed that arsenate adsorption was endothermic. The kinetic model corresponded to the pseudo-second-order model. The Langmuir adsorption isotherm was better fitted to the experimental data. The Fe2O3/Al2O3 adsorbent was immobilized on leca granules and applied for As (V) adsorption. The results showed that the immobilization of Fe2O3/Al2O3 on leca particles improved the As (V) removal efficiency.