This study describes the gas chromatography–mass spectrometry (GC–MS) analysis of trace-level “air toxics” in humidified cannister air, using cryogen-free preconcentration technology. We show that this method is able to detect 65 target compounds ranging from propene to naphthalene, with method detection limits as low as 0.7 pptv in SIM mode, making it compliant both with standard TO-15 methods, and with “trace TO-15” methods stipulating lower detection limits.