An in situ regeneration of activated carbon bed using an ozonated water was studied in order for avoiding the carbon loss, contaminant emission and time consuming for discharge-regeneration-repacking in a conventional thermal regeneration process. Using phenol and polyethylene glycol (PEG) as adsorbates, the adsorption breakthrough and in situ regeneration with the ozonated water were repeated. These organics were supposed to degrade by the oxidation reaction of ozone, regenerating the bed for reuse. As the number of regeneration increased, the adsorption capacity for phenol was reduced, but the change was stabilized showing no further reduction after reaching a certain degree of decrement. The reduction of adsorption capacity was due to the increase of pore size resulting in the decrease of specific surface area during ozonation. The adsorption capacity of phenol decreased after the ozonated regeneration because the in-pore adsorption was prevalent for small molecules like phenol. However, PEG did not show such decrease and the adsorption capacity was constantly maintained after several cycles of the ozonated regeneration probably because the external surface adsorption was the major mechanism for large molecules like PEG. Since the reduction in the pore size and specific surface area for small molecules were proportional to the duration of contact time with the ozonated water, careful considerations of the solute size to be removed and controlling the contact time were necessary to enhance the performance of the ozonated in situ regeneration of activated carbon bed.