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

Abstract

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-methylhydroxylamine 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.