RI 7124 Analysis Of Mineral Matter In Coals By X-Ray Fluorescence

The Bureau of Mines has investigated the mineral matter content of 38 American coals using X-ray fluorescence. Measurements of the Ka intensity for magnesium, aluminum, silicon, sulfur, calcium, and iron permit the determination of those elements as well as an indirect determination of the ash con-tent of the coals. The percentage of each of the six elements was corrected for absorption by all six elements as well as by hydrogen, carbon, nitrogen, and oxygen. It made little difference whether the values used for hydrogen, carbon, and nitrogen were obtained from chemical analysis or whether average values for all coals were used. In all cases, oxygen was obtained by difference. The correction for absorption by all these elements involved the inversion of a 6 X 6 matrix and was performed by computer. Assuming that the elements magnesium, aluminum, silicon, calcium, and iron were present in the ash as oxides, the quantity of ash was determined. The results for the mineral elements as well as for ash and oxygen were in good agreement with chemical results. Particle size was found to have a significant effect on fluorescence intensities. A study of size effects was made for pyrite particles, since the sulfur content of coals is of particular interest. Theoretical equations were derived and verified relating the intensity to particle size. It was found that the coal samples must be ground to less than 2 microns. Sulfur appears in several forms in coal, and the effect of sulfur form on intensity was investigated. It was found that the Ka intensity was independent of sulfur form but the Kß intensity varied with the type of sulfur. Thus, the Ka intensity was used for determination of the quantity of sulfur present. Utilization of the sulfur KB intensity did not permit a determination of the proportions of sulfur forms present in coal. However, for synthetic mixtures of cystine and pyrite in carbon black, measurement of sulfur Ka and Kß permit determination of each constituents from measurements of sulfur intensities alone.