This paper describes activation of pine cone with Fenton reagent and determines the removal of Cd(II) and Pb(II) ions from aqueous Solution. Changes of the Surface properties of adsorbent materials were determined by the FT-IR and SEM analysis after activation of pine cone. The effect of Fe2+/H2O2 ratio, ORP, pH and contact time were determined. Different adsorption isotherms were also obtained using concentrations of heavy metal ions ranging from 0.1 to 150 mg L-1. The adsorption process follows pseudo-first-order reaction kinetics and follows the Langmuir adsorption isotherm. The study discusses thermodynamic parameters, including changes in Gibbs free energy, entropy, and enthalpy, for the adsorption of Cd(II) and Pb(II) on activated cone, and revealed that the adsorption process was spontaneous and exothermic under natural conditions. The maximum removal efficiencies were obtained as 91% and 89% at pH 7 with 90 and 105-min contact time for Cd(II) and Pb(II), respectively. (c) 2008 Elsevier Ltd. All rights reserved.