Polyacrylonitrile (PAN) hollow fibers were pretreated with ammonium dibasic phosphate, then further oxidized in air, carbonized in nitrogen, and activated with carbon dioxide. The effects of oxidation time of PAN hollow fiber precursor on the microstructure, specific surface, pore size distribution, and adsorption properties of PAN-based activated carbon hollow fiber (PAN-ACHF) were studied in this work. Both of specific surface area and adsorption ratio to VB12 reach maximums when PAN hollow fibers are oxidized for 5 h in air. The adsorption ratios for creatinine are all higher than 90% over all oxidation time. After 5 h of oxidation, the number of pores on the surface obviously increases, and the pore size is uniform. After 7 h of oxidation, the number of macropores in PAN-ACHF increases. The dominant pore sizes of mesopores in PAN-ACHF range from 2 to 5 nm. (C) 2007 Wiley Periodicals, Inc.