A method for the simultaneous determination of 1,4-dioxane, epichlorohydrin, 2-methylisoborneol (2-MIB) and geosmin in water by headspace solid-phase microextraction (SPME)-gas chromatography–mass spectrometry (GC/MS) is described. A carboxen (CAR)/polydimethylsiloxane (PDMS) SPME fiber was chosen. The small pores in carboxen particles make this carbon molecular sieve particularly effective for extracting small molecules, like 1,4-dioxane and epichlorohydrin. This method achieved one tenth of the regulated concentration values required in Japanese water regulation, and provided good repeatability with RSD values of between 2.0 and 7.7% at the concentration. The method provided linear ranges from 1 to 100 μg L
−1 for 1,4-dioxane, 40 to 4000 ng L
−1 for epichlorohydrin, and 1 to 100 ng L
−1 for 2-MIB and geosmin. The extractabilities of 1,4-dioxane, epichlorohydrin, 2-MIB and geosmin from a tap-water sample spiked at 10 μg L
−1, 400 ng L
−1, 10 ng L
−1 and 10 ng L
−1, respectively, were between 95.7 and 104.6% with RSD values of between 1.4 and 2.4%.
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