It gives immense pleasure to place before a large community of pharmacy students, my humble work on “INSTRUMENTAL METHODS OF ANALYSIS – A LABORATORY GUIDE” written in accordance with the recent syllabus prescribed for the B.Pharmacy students. It is hoped that the book will be received favourably as an effective practical book by both students and faculty of pharmacy. The book is a simple, handy, comprehensive and profusely illustrated digest on Pharmaceutical Analysis with special stress on the requirement of undergraduates. The realization of the need and importance for students promoted me to write new book as per syllabus of PCI semester pattern. It is also hoped that it will serve as a useful resource for teachers of Pharmaceutical Analysis. The major thrust has been to make the book more students friendly. The practical contents of the book are vital in the field of pharmaceutical sciences. Experiments have been explained according to the syllabus. The structure of this book is simple, self-explanatory and easy for the readers to grasp the subject.