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The most commonly used method for analysis of airborne carbonyls is to collect the analytes on solid sorbents coated with a suitable derivatization agent, followed by solvent desorption and liquid injection for analysis by high-pressure liquid chromatography. We have explored a new approach by combining on-sorbent derivatization and thermal desorption to measure airborne carbonyls. More specifically, carbonyls in the air are collected onto an O-(2,3,4,5,6−pentafluorobenzyl)hydroxylamine (PFBHA)-coated Tenax sorbent packed in a tube with dimensions identical to those of a gas chromatography (GC) injector liner. The derivatives are then released by in-injection port thermal desorption to a GC column for analysis. Gaseous carbonyls, including formaldehyde, acetaldehyde, benzaldehyde, glyoxal, and methylglyoxal, at ppbv levels are shown to be effectively collected (≥92% collection efficiency) onto the …