Samples of coal weighing approximately 200 g placed in a collimated beam of neutrons from the thermal column of the Ames Laboratory Research Reactor produce capture gamma-rays which can be used for the determination of sulfur in the presence of iron, a potential source of interference. Spectra from NaI(Tl) detectors were used with the help of Ge(Li) spectra to locate interferences. Corrections for iron interference was made by the use of a higher energy iron peak. A linear relation was found between the area of the hydrogen capture peak at 2.23 MeV and the amount of water added to coal.