A procedure has been worked out for isolation and determination of volatile organic sulphur compounds in water. These compounds are isolated from an aqueous sample by countercurrent thin-layer head-space (TLHS) technique. After isolation, the sulphur compounds are burned in a quartz tube and the combustion products (SO2/SO3 mixture) are absorbed by a 10% solution of hydrogen peroxide. The resulting sulphuric acid is introduced into the heated part of a quartz tube, where the presence of tungsten trioxide at 1150°C ensures its complete decomposition. The sulphur dioxide formed is titrated microcoulometrically with iodine. Organic halogen compounds usually present in different waters do not interfere. The complete procedure has been tested on model solutions of sulphur compounds in the concentration range of 10–200 μg S/l.