Magnetite nanoparticles (Fe3O4), with an average size of about 10 run, were encapsulated with polystyrene using a new method based on emulsifier-free miniemulsion polymerization in the presence of 2, 2' azobis (2-amidinopropane) dihydrochloride (V-50) as a cationic ionizable water-soluble initiator and hexadecane as a hydrophobe. Transmission electron microscopy (TEM) proved the presence of magnetite in polymer particles which appeared to be monodisperse in size, approximately 100-300 nm in diameter, through TEM and scanning electron microscopy (SEM). Thermogravimetric analysis (TGA) measurement was used to determine the percentage of magnetite in the products. The results of emulsifier-free miniemulsion polymerization were compared with those of conventional emulsifier-free emulsion polymerization using (V-50) as the initiator in both cases. (c) 2005 Elsevier B.V. All rights reserved.