This laboratory manual provides a comprehensive introduction to an array of important techniques for polymer synthesis and characterization. The experiments are designed to be completed in one laboratory period using limited quantities of materials to reduce the costs and disposal problems, and were reviewed for classroom use at Polytechnic University. Students will benefit from the clear writing style and straightforward approach to concepts and procedures, while more advanced readers will appreciate the emphasis on fundamental principles and references to more in-depth explanations of the techniques. Polymer Synthesis and Characterization will serve as a unified laboratory manual for university courses as well as professional training courses in polymer science.