Coals research sample preparation

The support of H. R. Brown, Chief of the Division of Coal Research, C.S.I.R.O., is gratefully acknowledged. J. F. Corcoran prepared many of the samples used for electron microscopy. 

It is the purpose of this chapter to present some indication of the spectroscopic methods that have been applied to coal analysis (Vorres, 1993, and references cited therein under the specific spectroscopic method). However, the standard test methods are not in any great abundance, but that does not stop the researcher for making such a request of the analyst for spectroscopic analysis. Thus, reference to the scientific literature is necessary, keeping in mind that the focus of the references is the description of the technique and that sample preparation and sampling are of the utmost importance. 

All analyses of Antarctic coal samples submitted from the U.S. Geological Survey have been analyzed at the U.S. Bureau of Mines, Coal Analysis Section under supervision of Forrest E. Walker. Preparation of samples for analyses as well as field sampling and shipment was supported, in part, by NSF grant G-17216 administered by the Institute of Polar Studies through the Research Foundation, The Ohio State University. 

Chemical analyses by INAA were conducted at the Archaeometry Laboratory at the Missouri University Research Reactor Center (MURR). Aliquots of sample were oven-dried at 100 °C for 24 h. Amounts of approximately 150 mg were weighed into small polyvials used for short irradiations. At the same time, 200 mg of each sample was weighed into high-purity quartz vials used for long irradiations. Along with the majolica samples, reference standards of SRM-I633a (coal fly ash) and SRM-688 (basalt rock) were similarly prepared, as well as quality control samples of SRM-278 (obsidian rock) and Ohio Red Clay (standards treated as unknowns). 

We are indebted to G.R. Dyrkacz and his collaborators and to R.E. Winans and K.L. Stock for the preparation of the macerals used in this study. The research was supported by the Department of Energy. The whole coal samples were provided by W. Spackman from the Pennsylvania State University Coal Sample Bank. 

The authors are indebted to R. W. Sanders, M. R. Smith, J. H. Reeves, C. L. Nelson, and M. R. Grove for their assistance with the analyses. E. S. Getchell, R. M. Garcia, and G. M. Garnant provided assistance with preparation of the manuscript. We are also indebted to the staffs of the Laramie Energy Research Center, Lawrence Livermore Laboratory s Oil Shale Project, the Pittsburg and Midway Coal Company, and Phyllis Fox of the University of California, Berkeley, for providing us with samples. This research was supported by ERDA Contracts RPLS-2126 and RPLS-1654. 

The test material used In these experiments was CRM-1, a coal-oll comparative research material obtained from Oak Ridge National Laboratory. CRM-1 Is a liquid product from the SRC-II (solvent-refIned-coal-II) process and Is a mixture of middle and heavy distillates In a ratio of 2.9 to 1. Aqueous solutions of the test material were prepared by stirring crude CRM-1 with distilled water In 1-gal solvent bottles at a level of 2 g/L for five days. After equilibration, undlssolved oil was removed by passing the sample through a coarse glass frit, followed by filtration through a 0.45-U membrane filter three times to ensure a true aqueous solution with no visible droplets of undlssolved oil. 

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