This study deals with the surface fluorination of poly(phenylene oxide) (PPO) with the direct contact of 100 ppm fluorine gas. To characterize the surface fluorinated membranes, the contac angle measurement, X-ray photoelectron microscopy analysis and the gas permeation experiments were performed. As the fluorination time increases, the hydrophobicity of membrane surfaces is increased by the surface characterization. In general, as expected, the overall gas permeability was reduced. Typically, the permeability reduction of 33% for nitrogen, 23% for oxygen and 3% for carbon dioxide were observed when the membranes were exposed in 100 ppm environment for 60 min., meanwhile the selectivity was increased from 3.92 to 4.47 for $O_2/N_2$ and 18.09 to 25.4 for $O_2/N_2$, respectively.