Solid phase microextraction (SPME) combined with TGA as a technique for guest analysis in crystal engineering

Abstract

A method has been developed to extract evolved guest molecules from a TGA exhaust stream using solid phase microextraction fibers (SPME). The study was conducted using a known hydrogen bonded framework consisting of Zn(HPDCA)₂·(H₂O)₂ and o-tolidene which has been shown to contain guest molecules. These guests co-crystallize inside the 1-D channels formed during the self-assembly of the hydrogen bonded framework. Single guest as well as mixed-guest-containing host frameworks have been analysed using this method. Guest molecules extracted in this fashion were successfully characterized using gas chromatography and mass spectrometry without the necessity of coupled TGA/GCMS.