Based on the authors’ extensive experimental experience, NMR Spectroscopy of Polymers explains the practical use of NMR spectroscopy in polymer chemistry. This laboratory manual first briefly introduces the basic principles of NMR and considers the key issues of accuracy and precision of the NMR measurements for the analysis of polymer structure such as tacticity, copolymer composition, chain end structures, and volume magnetic susceptibility by NMR. Successive chapters then address stereochemistry of polymer chains, chemical composition and sequence in copolymers, polymerization reactions, two-dimensional NMR spectroscopy, NMR relaxation, and the promising combined use of spectroscopy and chromatography. The book can serve not only as a reference for experienced NMR users but also as an introduction for newcomers.