A series of poly(ethylene-co-vinyl acetate-co-carbon monoxide) terpolymer samples with varying monomer compositions were studied using a variety of one- and two-dimensional nuclear magnetic resonance (NMR) techniques at 750 MHz. Samples were characterized in deuterated),4-dichlocrobenzene-d(4) at high temperature (120 degrees C) to overcome the signal loss and broadening due to T-2 relaxation. Identification of major triads formed due to the addition of the three monomers in different permutations was facilitated by the use of different 2D techniques such as gradient assisted heteronuclear single-quantum correlation (gHSQC, gradient selected heteronuclear multiple-bond correlation (gHMBC), and gradient assisted HSQC-TOCSY. Detection of unusual structures formed due to the addition of carbon monoxide to vinyl acetate or structures due to the inversion of vinyl acetate was also possible. Because of improved dispersion the study was not restricted to the triad level, but in some cases pentads could also be identified. Distinct resonances of chain ends and short-chain branches were also observed.