Several raw coals of various ranks were used to examine the effects of some of the variations in ASTM procedures on analytical results obtained for total sulfur and sulfur forms. ASTM procedures were also used to determine pyritic sulfur in two coals cleaned by selective agglomeration processes. In addition, organic sulfur values obtained by the indirect ASTM procedure were compared to those obtained directly by leaching coal with hot HNO3 followed by total sulfur determinations on the coal residue. Differences in the ASTM leaching procedure with HNO3 did not significantly affect the pyritic sulfur results for any of the coals. However, small differences between the referee (leaching coal with HNO3) versus alternate (leaching coal ash with Hcl) ASTM procedures for determining pyritic sulfur were observed. Neither procedure was consistently higher than the other. Based on analytical variations observed for pyritic, sulfate, ana total sulfur for a given coal, ASTM organic sulfur values varied by 20-40% (relative), depending on which values were used to calculate the organic sulfur by difference. Organic sulfur values obtained directly were slightly lower than the ASTM organic sulfur values for three of the five coals examined. The organic sulfur values obtained directly were an average of 0.2% (absolute) lower than those obtained indirectly. Differences in values determined directly versus indirectly may be coal specific.