Abstract: | The microstructure of trans‐4‐methacryloyloxyazobenzene–methyl methacrylate copolymers prepared by solution polymerization process using AIBN as initiator is analyzed by one‐and two‐dimensional spectroscopy. Sequence distribution was calculated from the 13C(1H)‐NMR spectra of the copolymers. Comonomer reactivity ratios were determined using the Kelen–Tudos and the nonlinear error‐in‐variables methods are rA = 1.14 ± 0.08 and rM = 0.51 ± 0.03; rA = 1.13 ± 0.1 and rM = 0.50 ± 0.04, respectively. The sequence distribution of A‐ and M‐centered triads determined from 13C(1H)‐NMR spectra of copolymer is in good agreement with triad concentration calculated from a statistical model. The 2‐D heteronuclear single‐quantum correlation and correlated spectroscopy (TOCSY) was used to analyze the complex 1H‐NMR spectrum. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 74: 3016–3025, 1999 |