A simple gas chromatographic method for the determination of residues of a fumigant mixture of chloroform, carbon tetrachloride, trichloroethylene, and carbon disulfide, applied in a liquid admixture to cereal grain, is described. Fumigated samples were submitted to stead distillation in the presence of toluene and an aliquot of the toluene layer was injected into the gas chromatograph. Nanogram quantities of mixture components were determined using an electron-capture detector.