SYNOPSISRelatively uniform polymeric microspheres, the coefficients of variation being close to lo%, were obtained by the BPO-initiated suspension polymerization of styrenic monomers. Unlike the conventional stirred-tank system, a particular microporous glass membrane ( SPG ) provided uniform monomer droplets continuously when monomer was allowed to permeate through the micropores. The monomer droplets were suspended in an aqueous solution containing the stabilizing agents, transferred to a stirred vessel, and polymerized. Up to 10 pm spheres, of a far narrower size distribution than those obtained by conventional microsuspension polymerization spheres, were obtained. The initial droplet size and distribution were retained with the successful suppression of secondary particle nucleation by the addition of hydroquinone in the aueous phase. Crosslinked polystyrene spheres were also synthesized in the presence of various low-molecular-weight diluents. While a good solvent, toluene, was not so effective; poor solvents, n-hexane and n-heptane, easily yielded the microporous structure, the specific surface area being as high as 160 m2/g.