Methacrylonitrile-vinylidene chloride (M/V) copolymers of different composition were prepared by bulk polymerization using benzoyl peroxide as an initiator under nitrogen atmosphere in a sealed tube. The copolymer composition was determined from quantitative C-13[H-1] NMR spectra. The reactivity ratios for M/V copolymers obtained from a linear Kelen-Tudos method and nonlinear error-in-variables method are r(M) = 2.47 +/- 0.14, r(V) = 0.40 +/- 0.02, and r(M) = 2.43, term of compositional and conformational sequences of these copolymers were done with the help of distortionless enhancement by polarization transfer, two-dimensional heteronuclear single-quantum coherence spectroscopy. (c) 2005 Wiley Periodicals, Inc.