Four series of activated carbons prepared from lignocellulosic materials (almond shells and olive and peach stones) by either physical activation—gasification (uncatalysed and iron catalysed) in CO 2 or in a water-nitrogen mixture—of chars or direct chemical activation with ZnCl 2 of the precursor were selected to show the comparative behavior of the activation procedures. Activation with CO 2 opens and widens the microporosity of the char with even a shift to meso- and macroporosity, the ablation of the exterior of the particle being very important at high burn-off; the final activated carbon has a well developed micro- and macroporosity, with a relatively small contribution of mesoporosity. The iron catalysed CO 2 gasification and gasification with water-nitrogen mixture produce carbons with a well developed macroporosity, although the latter has the advantage of maintaining a well developed micro- and mesoporosity. Direct chemical activation of the precursor with ZnCl 2 produces, in only one step, a larger yield of activated carbon having microporosity as well developed as in the CO 2 gasification of the char, with the advantage of producing a much larger mesopore volume.