This paper reports NiO as a novel and an efficient adsorbent for the removal of Pb from aqueous solutions. In the present investigation. Pb adsorption experiments on NiO were conducted on aqueous solution at different initial Pb concentration, pH of the solution and adsorption temperature. The mechanism of adsorption was observed to be an ion exchange between the surface proton and Pb in aqueous solution. Experimental data were best described by the Langmuir isotherms. The surface structure of the NiO before and after adsorption of Pb was analyzed by using FTIR spectroscopy, scanning electron microscopy (SEM) coupled with energy dispersive X-ray analyses (EDX). (C) 2009 Elsevier B.V. All rights reserved.