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Phase separation by semi-interpenetrating polymeric network formation based on the copolymer styrene-divinylbenzene (PS-DVB) and poly(buty1 methacrylate) (PBMA) was investigated by light scattering. The time for phase separation was measured as a function of the rate of the copolymerization reaction and of the composition of the initial blend. The time until the outset of phase separation decreases with increasing content of PBMA in the blend. The change in concentration of DVB does not influence the process of phase separation.