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The book provides a concise and practically-driven overview of fundamentals and current experimental practices in the field of characterization of modern polymer, biopolymer materials and related composites. Such guide is important for experienced undergraduate students and new graduate students starting their adventure into polymer materials research. It helps students with quick introduction into theoretical basics, guidance on experimental routines, specimen preparations, data analysis, resolution and limitations of experimental measurements, and common issues and artifacts. It includes most popular spectroscopic and microscopic techniques for understanding chemical composition, microstructure and morphology, and fundamental properties of solid polymeric materials including mechanical, viscoelastic, thermomechanical, surface, and optical properties. All chapters are accompanied by examples of specific study cases, experimental problems and questions for solving and self-testing, as well as laboratory practice videos collected by the authors in their labs.