Iodine-doped activated carbon fibers (ACFs) were prepared by the iodine immersion method on pitch-based ACE Then iodine-doped ACFs were heated in argon at 523 K for 4 h and at 673 K for 2 h. The iodine structure of the resultant iodine-doped ACFs was examined using X-ray photoelectron spectroscopy. The micropore structures were determined by N-2 adsorption at 77 K. The surface area and micropore volume of iodine-doped ACFs are less than those of pristine ACFs. However, the pore width does not change with the iodine doping. The effects of iodine doping on adsorption properties of ACFs for H2O and NO at 303 K were examined. The iodine doping affected remarkably the adsorptivities of ACFs for H2O and NO. In particular, iodine-doped ACFs treated at 673 K show enhanced adsorptivities for H2O and NO. This result suggests that iodine molecules doped on the micropores should be charged by heat treatment at 673 K.