Poly(glycidyl methacrylate) and water-soluble copolymers of glycidyl methacrylate with N-vinylpyrrolidinone were prepared by free-radical-initiated solution polymerization in chloroform. Polymer microstructure was investigated by high-field H-1 and C-13 nuclear magnetic resonance (n.m.r.), H-1 decoupled C-13 n.m.r., H-1-C-13 correlation n.m.r. and 135 DEPT (distortionless enhancement by polarization transfer) n.m.r. The combined use of these techniques allowed unequivocal C-13 and H-1 n.m.r. assignments of carbons and protons to be established. Copolymer composition was thus determined from H-1 n.m.r.