Poly(vinyl alcohol) (PVA) coating solution containing glutaraldehyde (GA) and maleic anhydride (MA) ascrosslinking agents was coated onto hydrolyzed poly acrylonitrile (PAN) hollow fiber membranes. The permselectivities ofthe resulting composite membranes prepared varying the reaction temperature and the concentration of the crosslinkingagents were tested for 90 wt% ethanol aqueous mixtures by the pervaporation technique at 60°C. In general, the flux decreasedwhile the selectivity increased for the increases of the reaction temperature and the crosslinking concentration. Incase of GA as a crosslinking, the flux 165 g/m²hr and the separation factor 81 were obtained at GA 11 wt% and the reactiontemperature 120°C. And for the case of MA, the flux 174 g/m²hr and the separation factor 73 were obtained at MA11 wt% and the reaction temperature 120°C.