Polymerization inhibitors and promoters for unsaturated polyester resins; use of solid phase microextraction and gas chromatography coupled to mass spectrometry for the determination of 4-tert-butyl catechol and acetylacetone

This paper reports a contribution of three on-sample derivatization sampling techniques for acetylacetone, 4-tert-butyl catechol and its oxidated derivatives 4-tert-butyl-1,2-benzoquinone determination in unsaturated polyester resins. The use of O-(2,3,4,5,6, pentafluorobenzyl)-hydroxylamine, trimethyloxonium tetrafluoroborate and O-methyl-hydroxylamine is combined with automated head space/solid phase microextraction and gas chromatography/mass spectrometry analysis. For an innovative powerful meaning in high-throughput routine, the generality of the structurally informative mass spectrometry fragmentation patterns together with the chromatographic separation are also investigated. The detection limits for these polymerization inhibitors and promoters are less than 27 pg for one mg of unsaturated polyester resin. In this study a new autosampler platform is proposed by using the Multi Fiber Exchange device in a xyz robotic system. We promote these methods as the analytical reference in the polyester resin field. The introduction of dedicated, automated, and robotic systems allowed a friendly use of MS apparatus for high-throughput screening and it reduces the costs of monitoring campaigns.