Abstract: Several different types of alkyd resins have been analyzed by simultaneous pyrolysis methylation gas chromatography -mass spectrometry (SPM-GC-MS). The sample was mixed with tetramethylammonium hydroxide, and the process included simultaneous pyrolysis derivatization and mass spectrometry determination. The identification of dibasic acid, polyol, drying oil type, and rosin and acrylic modified alkyd. This method is sensitive, accurate, convenient, and involves minimal sample manipulation.