Copolymers of N-vinylcarbazole and methyl methacrylate of different compositions were prepared by solution polymerization with azobisisobutyronitrile as an initiator, and their compositions were determined from quantitative C-13{H-1}-NMR spectroscopy. The reactivity ratios for the comonomers were calculated with the Kelen-Tudos and nonlinear error-in-variable methods. The complete spectral assignment of the overlapping H-1 and C-13{H-1} spectra of the copolymers was made with the help of distortionless enhancement by polarization transfer, two-dimensional heteronuclear single-quantum correlation, and total correlation spectroscopy. (C) 2003 Wiley Periodicals, Inc.