Viscose fibre based materials were carbonized and activated using CO2 as an activation agent. Materials were pretreated with fire retardants and activated at 900°C. Degree of activation varied from 5 to 75%. Sample size was from 100 mg to 8000 g. Optimization of a pilot scale activation process was done with a number of laboratory scale experiments. The samples produced were characterized by nitrogen adsorption techniques. The results were used for surface area and pore volume determinations. In addition the samples were characterized by adsorption of different organic adsorbates from vapour phase. Vapour phase adsorption determinations were carried out by measuring adsorption capacities at saturated vapour (single point) pressure at constant temperature.