In this work, carbon xerogels with a high pore volume and surface area (up to 2.58 cm 3 /g and 3200 m 2 /g respectively) have been synthesized using the sol-gel polycondensation of resorcinol (R) with formaldehyde (F) in a basic medium of monoethanolamine (MEA), followed by drying and pyrolysis. This medium (MEA) has not been used in previous investigations. The effect of activation with CO 2 on the pore size distribution and the chemical functional groups has been investigated using N 2 (77 K) adsorption, FTIR and elemental analysis techniques. A series of experiments has been conducted to investigate the effect of activation time and activation temperature. Activation of the samples was carried out at 850, 900 and 980°C for times ranging from one to three hours. Within the range of activation conditions, an increase in activation time at 850°C results in a continuous steady rise of the BET surface area and total pore volume. However, at the two higher temperatures, the surface area shows a maximum when plotted against activation time. FT-IR results show that the use of MEA as a catalyst leads to the formation of nitrogen functional groups in the surface of the resin.