Abstract: | 4‐Vinyl pyridine–methacrylonitrile (V/M) copolymers of different composition were prepared by bulk polymerization using benzoyl peroxide as an initiator. The copolymer composition was determined from quantitative 13C{1H}‐NMR spectra. The reactivity ratios for V/M copolymer obtained from a linear Kelen‐Tudos method (KT) and nonlinear error‐in‐variables method (EVM) are rV = 0.79 ± 0.12, rM = 0.38 ± 0.09 and rV = 0.79 ± 0.13, rM = 0.38 ± 0.07, respectively. The complete spectral assignment in term of compositional and configurational sequences of these copolymers were done with the help of distortionless enhancement by polarization transfer (DEPT), two‐dimensional heteronuclear single quantum coherence spectroscopy (HSQC). Total correlated spectroscopy (TOCSY) experiment was used to assign the various three‐bond 1H‐1H couplings in the V/M copolymer. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 3232–3238, 2003 |