A new coupling of organic elemental analysis with flame photometric detection (OEA-FPD) was developed for the determination of total sulfur at nanogram levels. The method is based on the combustion of the sample under oxygen at high temperature, further reduction of the gases released, chromatographic separation and photometric detection. Combustion, chromatographic detection and coupling conditions are described and optimized. The new system is completely automated and fast (5 min per sample) and provides good accuracy, sensitivity and precision [reproducibility (RSD) < 7.5%]. Limits of detection were for solids 1.2 ng S and for liquids 0.2 ng S. The method was applied to a wide range of solid and liquid samples. Up to 125 analyses can be carried out without changing the combustion reagents.