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The various techniques used to analyze the microstructures of polymers are presented in this book. High resolution and solid state techniques are described, and applications to both synthetic and biological polymers are discussed in detail. Particular emphasis is placed on the determination of polymer microstructure by NMR spectroscopy. Here attention is drawn to the connection between the microstructures and NMR spectra of polymers, and it is demonstrated that the local polymer conformation provides this link. The numerous examples illustrating this connection are a special feature of the book.