Monodisperse poly(methylmethacrylate) microspheres having a diameter of 2.6 mu m and a molecular weight of 102.277 g/mol with 5.3% of the C-v (the coefficient of variation) were synthesized by the dispersion polymerization using hydrophilic polyvinylalcohol (PVA) in methanol/water mixture media. Then, the structural verification of the synthesized materials is confirmed by using H-1 NMR and FT-IR spectroscopy. The effects of PVA and the polymerization parameters such as the initiator, monomer and stabilizer concentrations. and the reaction time on the characteristics of the final particles were studied. Thus, the role of PVA in the dispersion polymerization of MMA is not only a steric stabilizer by physically adsorbed in methanol phase, but also a colloid protective to give relatively monodisperse polymer particles in water phase, simultaneously. (c) 2006 Elsevier Ltd. All rights reserved.