The organic chemist who wishes to learn how to use NMR spectra effectively must first learn the essential facts and then must gain both ability and confidence through the solution of a wide range of specific problems. My previous volume, Interpretation of NMR Spectra: An Empirical Approach, was written specifically to present and explain the necessary background material. The present volume is designed to provide the reader with a full range of experience in the interpretation of NMR spectra. The exercises are arranged in a sequence designed for rapid assimila tion of not only the basic concepts, but also increasingly more complex details. Emphasis is placed on the difficulties normally encountered in the use of spectra and also on the many practical aids which are helpful in overcoming these difficulties. For most of the problems, at least one reasoning process is outlined by which the questions can be answered. This text is, in part, an outgrowth of my participation in workshops which were held at Canisius College under the direction of Dr. Herman Szymanski and at the College of Pharmacy of the University of Illinois under the direction of Dr. Charles L. Bell v and Dr. Ludwig Bauer. This experience has been of considerable aid in the formulation of this workbook. Most of the spectra used in this book were obtained by Searle staff members in the course of their own research.