The volatiles of a flat-head, Calliurichthys doryssus, which gives out a characteristic offensive odor in living time, were analyzed by gas chromatography. 2. A large quantity of volatile sulfur compounds was detected in the flat-head; of which methyl mercaptan and/or dimethyl disulfide were judged to be responsible for the offensive odor. 3. The contents of methyl mercaptan and dimethyl disulfide were much higher in skin than in muscle and viscera.