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The potential of solid phase microextraction (SPME) for the determination of the soil fumigants 1,3‐dichloropropene (1,3‐DCP) and methyl isothiocyanate (MITC) in environmental samples such as soil and water samples has been investigated. Direct immersion SPME followed by GC/ECD/NPD analysis allowed the rapid determination of the two fumigants in water samples, with very little sample manipulation, giving an LOD of 0.5 μg L–1. Precision, calculated as relative standard deviation (RSD) for six replicates at three concentration levels, was found to be lower than 20% at the concentration levels tested. For the analysis of soil samples, headspace (HS)‐SPME combined with GC/ECD/NPD analysis has been applied. Quantification using matrix‐matched calibration curves allowed determination of both analytes (MITC and 1‐3‐DCP) with a LOD of 0.1 μg kg–1(RSD <10%) for the two concentration levels assayed (0.02 and 0.2 mg kg–1). The HS‐SPME procedure developed in this paper was applied to soil samples from experimental green house plots treated with metham‐Na, a soil disinfestation agent that decomposes in soil to MITC. The absence of sample manipulation as well as the low solvent consumption in SPME methodology are among the main advantages of this analytical approach.