Alumina hollow microspheres with high adsorption affinity toward p-nitrophenol in water were prepared by using urea and trisodium citrate as precipitating and mediating agents, respectively, via a simple one-pot hydrothermal synthesis followed by calcination. The as-prepared samples were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and nitrogen adsorption-desorption isotherms measurement. This study shows that the morphology, specific surface area, and the pore structure of the resulting materials can be controlled by varying the concentration of trisodium citrate. The result of adsorption of p-nitrophenol onto the as-prepared samples revealed that the pseudo-second-order kinetic equation can better describe the adsorption kinetics. Furthermore, adsorption isotherm studies indicated that the resulting alumina microspheres are powerful adsorbents for the removal of p-nitrophenol from water with maximum adsorption capacity of 217.4 mg/g. (C) 2012 Elsevier Inc. All rights reserved.