A recently develped analytical method using the EPM (electron probe microanalyzer) measures organic sulfur directly and avoids the uncertainty of calculating organic sulfur content by difference. Analysis of 18 different coals (from 10 states, ranging in rank from subbituminous C to low vol. bituminous, and in age from Pennsylvania to Palaeocene) shows that organic sulfur contents of coals can be calculated from the organic sulfur contents of the vitrinite in the coals. This empirical relationship exists because vitrinite is the dominant maceral type is most coals and generally has a sulfur composition intermediate between exinites and inertinites. For EPM organic sulfur analysis, representative samples (−20 to −60 mesh) are potted in 1″diameter epoxy pellets, polished and carbon coated. Vitrinite grains are identified during analysis by shape and texture, with results equivalent to oil immersion, reflectance techniques. According to t‐statistics, analyzing 15 vitrinite grains achieves a maximum variability of less than 0.20 wt % from the ’’true’’ organic sulfur content of coals containing less than 2.00 wt % organic sulfur. Neither operator experience nor variation in coal composition and rank appear to bias results. A mojor problem with the EPM technique has been finding a suitable EPM sulfur standard. Recently, in cooperation with L. A. Harris, Oak Ridge National Laboratory, we have prepared a good standard, derived from a petroleum coke, which is stable under an electron beam and contains a uniform sulfur content.