Total sulfur has been measured in 13 petroleum and 14 coal Standard Reference Materials (SRMs) by isotope dilution thermal ionization mass spectrometry. These materials are suitable as primary and quality control standards for determining the sulfur content of oils and coals by X-ray fluorescence and high-temperature combustion instrumentation. Samples were spiked with enriched stable 3% and combusted in sealed Carius tubes using nitric and hydrochloric acids. The oxidized sulfur was reduced to HzS, precipitated as AsBk and then dissolved in an ammoniacal solution of As2O3. A portion of this solution, equivalent to 1.5 pg of sulfur, was added to a single Re filament coated with silica gel. The amount of sulfur in the samples was determined from the j8/3% ratio by measuring the 75As3%+/75As3%+ molecular ions in a Faraday detector. A total of 158 sulfur procedural blanks covering a 10-year period show an approximate lognormal distribution with a grand mean of 0.26 pg of sulfur. This is a negligible correction for most of the data reported here. The total uncertainty (95% confidence interval) for homogeneous materials such as oils is about 0.5%, and for less homogeneous materials such as coals is 1-496.One of the most important properties of fossil fuels is their sulfur content. Combustion of fossil fuels is the primary source of anthropogenic sulfur compounds released into the atmosphere. Recent estimates suggest that the anthropogenic flux into the atmosphere may be equal to or greater than the natural flux. Electric utilities within the United States burn a large amount of fossil fuel and are responsible for approximately 70% of the SO2 emitted into the atmosphere.' After entering the atmosphere, oxides of sulfur are converted to sulfuric acid and sulfate particles. These particles play an important role in the physics and chemistry of the atmosphere. The radiation budget of the earth is influenced by the fine particles in the atmosphere. Visibility degradation resulting from sulfate aerosols has been of concern particularly in pristine areas such as national parks. Rollback in sulfur emissions from fossil-fueled power plants has been an environmental goal for the last two decades.The accurate determination of the concentration of sulfur in fossil fuels is important for several reasons. The quality and price of both petroleum and coal are related to the amount of sulfur present. There are federal, state, and local regulations This article not subject to US. Copyright. Published 1994 by the American Chemical Society that limit the amount of sulfur oxides that can be emitted during the combustion of fossil fuels. Electric power companies must monitor the emissions from their stacks in order to comply with regulations of the Environmental Protection Agency. These companies also closely monitor the sulfur content of their incoming feedstocks to ascertain the quality, acceptability, and price. The fossil fuel producers and users require fast and inexpensive methods for the determination of sulfur in the rangeof 1-5% ...