Carbon aerogels were prepared from Resorcinol/Formaldehyde (R/F) and Pyrogallol/Formaldehyde (P/F), dissolved in water, using sodium carbonate as a catalyst, water is interchanged with acetone and this with CO2 at 900 °C.The aerogels are activated with CO2.Aerogels were characterized by nitrogen adsorption of (N2) at -196 °C, thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and Acid-base titration.The Pb (II) and Ni (II) adsorption were evaluated by isotherms from a simple solution.The solids obtained through R/F reaction have a structure with a high surface, up to 1064 m 2 /g, pore volume up to 0.582 cm 3 /g and a surface chemical composition influenced by the obtaining method, the nature of the precursors, the catalyst and the activation atmosphere, while those of P/F show surface areas of 103.6m 2 /g maximum.The thermally-treated aerogels showed better properties and in all cases, selectivity towards the lead.