Monolithic carbon aerogels were obtained by carbonization of organic aerogels prepared by polymerization of resorcinol and formaldehyde under different conditions. Some carbon aerogels obtained were further CO2-activated. Samples were characterized by gas adsorption, scanning electron microscopy, high-resolution transmission electron microscopy, and mechanical tests. Benzene, toluene and xylenes were adsorbed from dry air by using carbon bed columns, obtaining the breakthrough curves. There was no correlation between the amount adsorbed at the breakthrough point and the volume of micropores narrower than 0.7 nm. Conversely, a good linear relationship between the amount adsorbed at the breakthrough point and the total micropore volume up to a mean micropore width of around 1.05 nm was found. In addition, the height of the mass transfer zone decreased with the mean width of the total micropores up to a value of around 1.05-1.10 nm. One of the best adsorbents obtained showed the lowest height of the mass transfer zone and one of the highest amounts adsorbed at the breakthrough point, either per mass or volume unit. However, it had a lower elastic modulus and compressive strength than other monolithic carbon aerogels, although its compressive strength Q MPa) was still high enough to use it in carbon bed columns. The sample with the best mechanical properties was a poorer adsorbent. Regeneration of the exhausted adsorbents allowed the recovery of the hydrocarbons adsorbed without any appreciable loss of adsorption capacity of the carbon bed.