AbstractIn this paper; we compare double hydrophobic polystyrene-b-poly(solketal methacrylate) (PS-b-PSMA) and amphiphilic polystyrene-b-poly(glyceryl methacrylate) (PS-b-PGMA) diblock copolymer membranes which are prepared by combining the block copolymer self-assembly in solution with a non-solvent induced phase separation (SNIPS). Diblock copolymers (i.e., PS-b-PSMA) were synthesized by sequential living anionic polymerization, whereas polystyrene-b-poly(glyceryl methacrylate) (PS-b-PGMA) were obtained by acid hydrolysis of the acetonide groups of the polysolketal methacrylate (PSMA) blocks into dihydroxyl groups (PGMA). Membrane structures and bulk morphologies were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM); respectively. The resulting PS-b-PGMA diblock copolymers produce an ordered hexagonal cylindrical pore structure during the SNIPS process, while membranes fabricated from the double hydrophobic (PS-b-PSMA) do not under similar experimental conditions. Membrane performance was evaluated by water flux and contact angle measurements.