A simple, automated method for the measurement of methyl mercaptan (CH3SH) and dimethyl sulfide (DMS) has been investigated. These two sulfur gases have strong and unpleasant odors. The collection and separation are performed in sequence with a single short column packed with silica gel powder. CH3SH and DMS are separated according to their desorption temperatures and introduced into a chemiluminescence cell in this order. These two gases emit strong chemiluminescence by reaction with ozone. The calibration curves obtained are linear, which is superior to flame photometric detection of these substances. The whole system, including a small cylinder for the carrier nitrogen, can be set in a portable box. The instrument is applicable to breath odor analysis, and automated measurement of room air can also be performed. In toilet air analysis, it was observed that levels of the sulfur gases increased after dark. With this instrument, sulfur gases at a ppbv level are successfully measured by a simple procedure without much interference.