In this book efforts have been made to systematically define and explain all the listed principles and experiments of IR, MASS, NMR, UV-Visible, and XRD spectroscopy. Each chapter possess an objective. Also, every principle or experiment incorporates definition in bold, introduction, sequential events, key concepts, tips for interpretation, examples of compounds for investigation, relevant spectra, and data interpretation. The book embodies maximum possible current advance experiments. To make the readers strongly connected with subject matter of spectroscopic experiments, book represents all the components/experiments in a classified manner and also all the important statements and key points are made bold. Apart from it, this book supports each and every principle, experiment or component with beautiful and actual possible images and diagrams. After, making a reading of each chapter readers can test their knowledge by solving the subjective problems, objective problems and problems related to spectral interpretation that are important for competitive examinations. This book is designed especially for the under graduate and postgraduate students, to assist in easy understanding of various theories, principles, instrumentations, applications, advancements and data interpretation of different analytical techniques like IR, MASS, NMR, UV-Visible, and X-Ray spectroscopy. Among undergraduates this book is beneficial for the students of B. Pharm., B.Sc. (Chemistry, Physics, Analysis, Pharmaceutical Chemistry, Pharmaceutical Analysis, Analytical Chemistry, Instrumental Analysis), and B. Tech. (Chemical Engineering). Among Post graduate students this book is helpful for M. Pharm. (Pharmaceutical Chemistry, Pharmacology, Pharmaceutics, Pharmaceutical Analysis, Medicinal Chemistry, Quality control, Quality Assurance, Regulatory Affairs and many more), M.Sc. (Chemistry, Physics, Analysis, Pharmaceutical Chemistry, Chemical Engineering, Biotechnology), M. Phil (Chemistry, Physics, Analysis, Pharmaceutical Chemistry, Chemical Engineering, Biotechnology, MRI), Pharm. D. Moreover research scholars of pharmacy, physics, chemistry, engineering and also idustry professionals may take the benefits through this book in easy also deep knowledge.