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. Includes long-lasting and in-depth research experience in the field of polymer characterization of a wide variety of polymers, biopolymers and composites. Contains guide to training, practical use, data analysis, limitations and resolution, common experimental routine parameters, and other practical considerations such as applicability in real lab environment. Includes examples of study cases, questions and problems for student self-testing and analysis. Includes examples of prominent artifacts and data corruptions and how to avoid and correct those. Shows practical lessons in the video collected by the authors with specimen preparation, experimental parameters selection, measuring process, and data collection, all in real-time.