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Electron probe microanalysis (EPM) for organic sulfur content can be performed easily on -20 to -100 mesh coal samples. Samples need only be mounted in epoxy and polished as coal samples are commonly prepared for petrographic examination. 15 areas within non-contiguous vitrinite grains are analyzed with the EPM. Without the need to produce a photomosaic, the organic sulfur content of vitrinite, and therefore of a coal, may be determined in less than 10 minutes. To test the EPM method coals were analyzed for which the ASTM organic sulfur values were corrected for unextracted iron. Such a correction would take into account the effect of any pyrite that remained unextracted following the ASTM Standard Method D2492-68. As shown from the data the EPM organic sulfur contents are very close to those of the corrected ASTM values. Using the EPM method, the potential exists to achieve very rapid, multiple organic sulfur analyses, which in turn will allow for rapid, detailed measurements of variations in organic sulfur content occurring across coal seams.
Analytical Methods for Coal and Coal Products, Volume III, is the third of a three-volume treatise that aims to provide a detailed presentation of what constitutes the first comprehensive reference work devoted exclusively to the subject of analytical methodology for coal and coal products. The three volumes have been divided into a total of twelve parts, each part containing several chapters devoted to a particular subject. The present volume deals with gases, waste products, by-products, environmental problems, and miscellaneous analytical problems, as well as special instrumental techniques for solving various problems. Because different aspects of a particular subject are frequently scattered through various chapters in the volumes, cross-references between chapters have been entered. In addition, the subject indexes have been made as detailed as was practical, and the reader will benefit from examination of pertinent subjects in the indexes of all three volumes. A careful reading of these volumes will show that definitive solutions are not yet available in a number of instances. There is a clear need for continued research on the fundamentals of analysis of coal and coal products, and the development of reliable and accurate analytical instrumentation, including on-stream applications.
This paper reports on petroleum coke that is stable under an electron beam and contains a uniform sulfur content. Hence, it is a suitable standard for analysis of organic sulfur content of coal. It should be as applicable for analysis of organic sulfur in other fossil fuels. This standard is available for distribution.
The overall objective of this project is to develop an analytical method to directly measure the forms of organic sulfur in coal. The method will provide a route to monitor the effectiveness of coal preparation research directed toward removal of organic sulfur in coal. The approach involves subjecting diluted coal samples simultaneously to an oxygen flow and a linear increase in temperature. Distinctive sulfur dioxide evolution patterns are observed among coals of different rank and between raw and treated coals. Assignments have been made relating each specific sulfur dioxide evolution to the non-aromatic organic, aromatic organic, and inorganic sulfur present in coals and treated coals. Work is progressing on schedule to optimize experimental conditions and to improve the efficiency of the controlled-atmosphere programmed-temperature oxidation (CAPTO) method by developing a multiple sample instrumental system.