Orthogonal experimental design (OED) was employed to study the influences of carbonization process on the transport properties of hollow fiber carbon membranes (HFCMs). The conjoint analysis method was applied for the statistical analysis of OED results, and the importance of the investigated carbonization parameters on the performance of carbon membrane was found to be: purge gas > final carbonization temperature > heating rate > final soak time. A high performance hollow fiber carbon membrane (HFCM-5) was prepared from the optimal carbonization process. The carbon membrane structure and morphology were characterized by a Fourier transform infrared spectroscopy and a scanning electron microscope. The influences of the operating parameters such as temperature, pressure, and stage-cut on the carbon membrane performances were investigated by the single gas and gas mixture tests.