Ethyl acrylate (E)/methyl methacrylate (M) copolymers of different compositions were prepared, and their compositions were determined with H-1 NMR spectra. The complete spectral assignments, in terms of the compositional and configurational sequences of these copolymers, were made with the help of distortionless enhancement by polarization transfer and two-dimensional heteronuclear single quantum coherence spectroscopy. The alpha-(CH3)M,-CH (E), -CH2, and)C=O carbons of both M and E units were found to be sensitive to various compositional and configurational sequences.