The aim of this book is to provide a practical and affordable general lab manual for undergraduate Instrumental Analysis (IA) course. After extensive experience in teaching IA laboratory course for a number of years, I have developed this lab manual in what I believe to be an improved version of an IA manual that is both concise and comprehensive. The factors I consider most important for an IA manual to be effective in teaching are as follows: 1) the instruments covered in the manual should follow ACS guidelines, and reflect new advances in the field of IA, while also addressing industrial needs; 2) experiments in the manual should address the basic principles of the instruments and help the students to understand the fundamental concepts and mechanisms of the instruments; 3) the manual should facilitate the instructor to cover lab processes from both theoretical and operational perspectives; and 4) the lab manual should be affordable, and meet the needs of majority of today's undergraduate chemistry and other multi-disciplinary (e.g. environmental science) programs. This manual provides the core essentials for the most common instruments recommended by ACS guidelines as well as those used in a traditional chemistry program. They are electrochemistry (Chapter 2), spectroscopy (Chapter 3, 4, 5, 6, 7), separation (Chapter 8, 9, 10). Hyphenated techniques (GC/MS, LC/MS and ICP/MS) are also included in relevant chapters. Traditional mass spectroscopy is not covered in separate experiments, but the basic principles are introduced in the experiments of the hyphenated techniques. A separate chapter covering basic statistics is provided at the beginning of the manual (Chapter 1). I strongly believe that some basic statistical principals and operations (e.g., linear regression) are critical for students to comprehend the course objectives, as it has become an ever-expanding and important aspect for IA courses. This also provides some buffer period for the lecture session to proceed ahead the laboratory session. All experiments in this manual have been carefully selected and developed to address the factors mentioned earlier with consideration of applicability to research. Unlike other similar manuals, which are simple collection of experiments, I tried to select the most applicable experiments with different level of difficulties. For most chapters, the three experiments (categorized as A, B and C) are chosen to represent three levels of difficulty with experiment A addressing the basic principles and instrumentation, B representing more advanced application and C involving more advanced knowledge of general chemistry. In addition, the experiments are selected to minimize the use of toxic, flammable, and expensive chemicals. However, training students to handle hazardous materials is one objective of this course, and instructors are expected to address safety issues whenever necessary. In addition, usage of expensive and less commonly available equipment is also minimized in this manual. I strongly believe that an IA textbook should cover both the theory and instrumentation of analytical techniques, while a general IA lab manual should focus on the basic principles of the instrumentation. In this manual, an introduction of the basic principles and instrumentation are provided for each type of analytical technique. Each introduction aims to bring forward new ideas on the terminology, formula, basic components of instruments etc., which are necessary for implementation of an experiment. The introduction sections are brief and therefore, cannot be used as sole source of theoretical background for any specific analytical technique. This requires students to refer to the textbook or other available hard-copy of electronic (e.g. internet) resources to understand the theory of the instrument for each experiment before attending lab.