Microbeads possessing amine functionality at the surface have been prepared by two methods : In the first method, poly(4-vinylpyridine/styrene) P(4VP/S) copolymer microbeads containing 13-69 mol % 4-vinylpyridine (4VP) were synthesized from the monomers. In the second method, animated polystyrene (PS) particles were prepared by postpolymerization reactions on cross-linked PS and polychloromethylstyrene particles to obtain poly(aminomethylstyrene/styrene) and polydiethylaminomethylstyrene particles, respectively. Scanning electronic microscopy of P(4VP/S) microbeads showed regular and spherical particles having a diameter between 80 and 200 nm depending on 4VP content. The chemical structure of the various particles made was studied using Fourier transform infrared spectroscopy, electron spectroscopy for chemical analysis (ESCA), and elemental analysis, whereas thermal properties were determined by differential scanning calorimetry and thermogravimetric analysis.