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Phase diagrams for PVC‐PMMA and CPE‐PMMA systems were determined by electron probe microanalysis in combination with scanning electron microscopy. Further the dehydrochlorination kinetics of chlorine‐containing samples was investigated by investigating the change of X‐ray radiation intensity of chlorine after isobar‐isothermal annealing of the polymer mixtures. The solubility of the mixtures was found to be affected by the degree of dehydrochlorination of the samples. The shape of the curve passes an extremum which is immediately connected with the dependence of the phase diagrams on dehydrochlorination kinetics. The effect of the conditions of mixture preparation on the compatibility of the components and the kinetics of the change of compatibility during annealing were determined. The thermally induced phase separation in the mixtures is shown to be caused by kinetic processes described.

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