Sodium maleate-vinyl acetate (NaM-VA) and maleic acid-vinyl acetate (MAc-VA) copolymers were synthesized and characterized and their aqueous solutions were kept at 25 and 100 C. The molecular weight (M W ) of the copolymers was measured after different times of storage by size exclusion chromatography, and IR spectra were recorded. At 100 C, NaM-VA showed a continuous decrease of MW, which can occur due to the chain breaking and=or chemical modification, while for MAc-VA copolymer a decrease was observed, followed by an increase of the apparent MW. This difference of behavior was attributed to some interchain chemical reactions. The decrease in the molecular weight of the two copolymers at 25 C was found to be less important than at 100 C.