Phenol-formaldehyde resins and a low-cost biomass residue, olive stones (OS), were used to prepare five activated carbons for CO 2 separation at atmospheric pressure, i.e., in post-combustion processes or from biogas and bio-hydrogen streams. Two phenolformaldehyde resins were synthesized: Resol, obtained by using alkaline environment, and Novolac, synthesized in the presence of an acid catalyst. Carbon precursors were prepared by mixing both resins with KCl or by mixing the Novolac resin with OS. The precursors were carbonized under an inert atmosphere of N 2 at different temperatures.The last stage in the synthesis of the adsorbents involved physical activation with carbon dioxide, which was carried out at different temperatures and burn-off degrees.Response surface methodology (RSM) is proposed as a tool for rapidly optimizing the activation parameters in order to obtain the highest possible CO 2 capture capacity of activated carbons. The optimum values of activation temperature and burn-off degree that maximize CO 2 uptake by the activated carbons at 35 ºC and atmospheric pressure were obtained within the experimental region. A value of CO 2 adsorption capacity of 9.3 wt.% was achieved. Activated carbons derived from Novolac phenol-formaldehyde * Corresponding author. Tel.: +34 985 119 090; Fax: +34 985 297 662 E-mail address: cpevida@incar.csic.es (C. Pevida) 2 resin type and from OS showed great potential as adsorbents for CO 2 capture at atmospheric pressure.