In this data book, both conventional Py-GC/MS where thermal energy alone is used to cause fragmentation of given polymeric materials and reactive Py-GC/MS in the presence of organic alkaline for condensation polymers are compiled. Before going into detailed presentation of the data, however, acquiring a firm grip on the proper understanding about the situation of Py-GC/MS would promote better utilization of the following pyrolysis data for various polymers samples. This book incorporates recent technological advances in analytical pyrolysis methods especially useful for the characterization of 163 typical synthetic polymers. The book briefly reviews the instrumentation available in advanced analytical pyrolysis, and offers guidance to perform effectually this technique combining with gas chromatography and mass spectrometry. Main contents are comprehensive sample pyrograms, thermograms, identification tables, and representative mass spectra (MS) of pyrolyzates for synthetic polymers. This edition also highlights thermally-assisted hydrolysis and methylation technique effectively applied to 33 basic condensation polymers.