Copolymers of isobutyl 4,4'-diphenylmethane dimethacrylate and divinylbenzene in the form of microspheres were obtained. For their preparation, the following techniques of heterogeneous polymerization were used: suspension polymerization, suspension- emulsion polymerization, and precipitation polymerization. Among the obtained microspheres, those synthesized by suspenson-emulsion polymerization were of a size suitable for high-performance liquid chromatography, whereas the product of suspension polymerization could be used as a packing material for gas chromatography. Their porous structure was studied in details. The influence of the polymerization technique on the particle size and morphology was examined. (C) 2004 Wiley Periodicals, Inc.