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Mixed matrix hollow fibers composed of multi-walled carbon nanotubes (MWCNTs) and polyetherimide (PEI) were fabricated. Pre-treatment of MWCNTs was carried out prior to the incorporation into the polymer matrix using a simple and feasible two stages approach that involved dry air oxidation and surfactant dispersion. The characterizations of the surface treated MWCNTs using TEM and Raman spectroscopy have evidenced the effectiveness of dry air oxidation in eliminating undesired amorphous carbon and metal catalyst while surfactant dispersion using Triton X100 has suppressed the agglomeration of MWCNTs. The resultant mixed matrix hollow fibers were applied for O(2)/N(2) pure gas separation. Interestingly, it was found that removal of disordered amorphous carbons and metal particles has allowed the hollow structures to be more accessible for the fast and smooth transport of gas molecules, hence resulted in noticeable improvement in the gas separation properties. The composite hollow fibers embedded with the surface modified MWCNTs showed increase in permeability as much as 60% while maintaining the selectivity of the O(2)/N(2) gas pair. This study highlights the necessity to establish an appropriate pre-treatment approach for MWCNTs in order to fully utilize the beneficial transport properties of this material in mixed matrix polymer nanocomposite for gas separation., (Copyright © 2012 Elsevier Inc. All rights reserved.)