Macroporous, monosized poly(meta-divinylbenzene) and poly(para-divinylbenzene) beads have been prepared by the two-step activated swelling method with toluene or 2-ethylhexanoic acid as pore-forming agents. The type of divinylbenzene isomer as well as the type of porogen has a large effect on both physical and chemical properties of the monodisperse beads. Large pores are obtained with 2-ethylhexanoic acid as porogen while beads prepared in the presence of toluene consist of only small pores and exhibit a shrinking behavior upon drying. The beads have considerable amounts of residual vinyl groups at the end of polymerization, as determined by bromination and Fourier transform IR analysis. The morphology and texture of the particles have been investigated by scanning electron microscopy and atomic force microscopy.