A new variation of off-line TG evolved gas analysis is reported here. Gas collection is done by inserting sample tubes filled with a suitable adsorbent, into the exhaust from the TG instrument. The following gas analysis is carried out by placing the sample tubes into a commercial thermal desorption unit which is coupled to a GC/MS. In this way, both a chromatographic separation of components as well as a mass spectral identification are obtained. Two examples from the analysis of production chemicals demonstrate the usefulness of this approach.