A series of perfectly alternating polyimide/ poly(dimethylsiloxane) microphase separated block copolymers ranging from 0-50 wgt. % poly(dimethylsiloxane) have been measured for permeability characteristics. The polyimide segment of the copolymers was based on oxydiphthalicdianhydride (ODPA) and 1,4-Bis(4-amino-1,1- dimethylbenzyl)benzene (Bis P). The polysiloxane was an aminopropyl terminated poly(dimethylsiloxane). Randomly segmented block copolymers of =20 wet. % poly(dimethylsiloxane) with different segment lengths were also studied, based on the same materials for the sake of comparison with the perfectly alternating versions of the same block copolymers. Permeability measurements were performed on tough, microphase separated, transparent films with O₂, N₂, CH₄, and CO₂ gases in that order. The effects of the chemical composition and block lengths on permeability coefficients and selectivity values were evaluated. The permeability of copolymer films to gases was found to be highly sensitive to the morphology of the copolymer. The morphology was found to be controlled by varying the amount and the segment length of each component and this allowed for fine control of the permeability characteristics. Conversely, the measurement of permeability characteristics can lead to more information about the morphology of complicated microphase separated block copolymers. / Master of Science