The free-radical solution copolymerization of isobutyl methacrylate with lauryl methacrylate in the presence of an inhibitor was studied with thermoanalysis methods. A set of inhibited polymerization experiments was designed. Four different levels of initial inhibitor/initiator molar ratios were considered. In situ polymerization experiments were carried out with differential scanning calorimetry. Furthermore, to determine the impact of the polymerization media on the rate of initiation, the kinetics of the initiator decomposition were followed with nonisothermal thermoanalysis methods, and the results were compared with in situ polymerization counterparts. The robust M-estimation method was used to retrieve the kinetic parameters of the copolymerization system. This estimation method led to a reasonable prediction error for the dataset with strong multicollinearity. The model-free isoconversional method was employed to find the variation of the Arrhenius activation energy with the conversion. It was found that robust M-estimation outperformed existing methods of estimation in terms of statistical precision and computational speed, while maintaining good robustness. (C) 2008 Wiley Periodicals, Inc.