Thermogravimetry (TG) coupled with sequential mass spectrometry (MS/MS) offers structural Identification of compounds evolving during thermally stimulated processes while maintaining temporal resolution between the two analytical procedures. MS/MS identification of coevolving compounds, combined with the weight-loss data obtained from TG, furnishes a means of delineating complex thermolytlc pathways. The compatibility of TG (a predominantly atmospheric pressure technique) with atmospheric pressure chemical Ionization (APCI) permits an interface that Is easily coupled and decoupled. The control of both Instruments and all data acquisition and analysis are performed by a common minicomputer, and this Integration permits a "user friendly" Interface between the two techniques.