The specificity and efficiency of procedures for fractionating total S into inorganic and organic constituents were evaluated by analyzing a series of known standards. Acid volatilization was specific for FeS. Chromium reduction recovered over 90% of the S from FeS, S0, and FeS2. Acetone extraction followed by chromium reduction of the filtrate was specific for S0. Hydriodic acid reduction recovered > 90% of the S from FeS, SO42−, and p‐nitrophenyl sulfate, an organic aryl ester sulfate analog. The Zn‐HCl reduction procedure is of questionable value, only partially recovering S from SO42−, S0, and FeS2. None of these procedures affected l‐methionine. Analyses were performed on both moist and oven‐dried peat from Big Run Bog, West Virginia. Oven‐drying of peat samples increased estimates of ester sulfate S and SO42−‐S and decreased estimates of carbon‐bonded S, which was calculated by difference.

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