The Bureau of Mines developed two methods for determining iron II and iron III in 2- to 5-mg samples of coal using electron paramagnetic resonance (epr) spectrometry. One method used solid coal samples; the other method used aqueous solutions. The method using solid samples was more simple, technically, but required the use of x-ray fluorescent analysis, or another independent method, for determining total iron in the samples, and the results were subject to some uncertainty. The method using aqueous solutions appeared capable of greater certainty and did not require additional methods of total iron analysis but was more involved procedurally. The coals analyzed were found to contain much more iron II than iron III.