Carbon hollow fiber membranes have been prepared by pyrolysis of a P84/S-PEEK blend. Proximate analysis of the precursor was performed using thermogravimetry (TGA), and a carbon yield of approximately 40% can be obtained. This study aimed at understanding the influence of pyrolysis parameters-end temperature, quenching effect, and soaking time-on the membrane properties. Permeation experiments were performed with N 2 , He, and CO 2 . Scanning electron microscopy (SEM) has been done for all carbon hollow fibers. The highest permeances were obtained for the membrane submitted to an end temperature of 750• C and the highest ideal selectivities for an end temperature of 700 • C. In both cases, the membranes were quenched to room temperature.