Carbon materials, including amorphous carbon, graphite, carbon nanospheres (CNSs) and different types of carbon nanofibers (CNFs) [platelet, herringbone and ribbon], were chemically activated using KOH. The pore structure of carbon materials was analyzed using N-2/77 K adsorption isotherms. The presence of oxygen groups was analyzed by temperature programmed desorption in He and acid-base titration. The structural order of the materials was studied by X-ray diffraction and temperature programmed oxidation. The morphology and diameter distribution of CNFs and CNSs were characterized by transmission electron microscopy. The materials were also characterized by temperature-desorption programmed of H-2 and elemental composition. The ways in which the different structures were activated are described, showing the type of pores generated. Relationships between carbon yield, removed carbon, activation degree and graphitic character were also examined. The oxygen content in the form of oxygen-containing surface groups increased after the activation giving qualitative information about them. The average diameter of both CNFs and CNSs was decreased after the activation process as consequence of the changes produced on the material surface. (C) 2010 Elsevier B.V. All rights reserved.