Three volatile organic compounds (benzene, cyclohexane, dichloromethane) were adsorbed onto activated carbon fiber cloth.1 H (MAS and PFG) NMR techniques were carried out and the signals were analyzed in terms of peak surface areas and shifts. These techniques were shown to be very useful for determining i) the intrinsic quantification of adsorbed molecules (VOC and/or water) in the porosity of the materials; the adsorption capacities ranged from 0.2 to 4 mol.kg -1 , ii) the mechanisms of interactions between adsorbed organic molecules and the carbon walls;