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Chemical kinetics on thermal decomposition of polystyrene was studied by integrating the non-isothermal differential and integral methods. For decomposition of polystyrene in environment with only nitrogen, a mass loss stage was found at 282.9oC to 398.2oC. The maximum mass-loss rate was at 372.4oC. Kinetic analysis results indicated that it is a first-order chemical reaction. Thermal decomposition of polystyrene was also investigated by the â€œpyrolysis gas chromatography mass spectrometryâ€ Py/GC/MS technology. Decomposition of polystyrene would be enhanced when the temperature increased. Upon heating by external sources, polystyrene would be decomposed to larger radicals. The large radicals would then produce smaller products through a series of reactions such as decomposition, radical recombination and hydrogen transfer.