Fumigant residues in hay were extracted by microwave irradiation. Hay, in gastight glass flasks, was placed in a domestic microwave oven, and fumigants were released into the headspace by microwave irradiation. Power settings for maximum release of fumigants were determined for carbonyl sulfide (COS), carbon disulfide (CS2), cyanogen (C2N2), ethyl formate (EF), methyl bromide (CH3Br), sulfuryl fluoride (SF), propylene oxide (PPO), and phosphine (PH3). Recoveries of fortified samples were > 91% for COS, CS2, CH3Br, SF, PPO, and PH3 and > 76% for C2N2 and EF. Completeness of extraction was assessed from the amount of fumigant retained by the microwaved hay. This amount was determined from further microwave irradiation and was always small (< 5% of the amount obtained from the initial procedure). Limits of quantification were < 0.1 mg/kg for COS, CS2, C2N2, EF, and PH3 and < 0.5 mg/kg for CH3Br, SF, and PPO. These low limits were essentially due to the absence of interference from solvents and no necessity to inject large-volume gas samples. The microwave method is rapid and solvent-free. However, care is required in selecting the appropriate power setting. The safety implications of heating sealed flasks in microwave ovens should be noted.