Three phases of work were performed for this study. First a new form of liberation analysis was created and applied to two coal samples from separate formations. This new method of liberation analysis attempts to remove sources of error found in the traditional form of liberation analysis. This new method is capable of producing results comparable to multiple iterations of the traditional liberation analysis while using only one head sample. The new method relies on the mathematical reconstruction of the data to produce the resulting liberation profile. This allows the user to easily expand the method to include more liberation profiles without greatly increasing the amount of head weight needed. The results of this phase confirm that the products of each liberation profile reconstitute the correct feed ash. The second phase of work focused on the evaluation and concentration of rare earth elements (REEs) present in the refuse streams of coal processing plants found in the eastern United States. Twenty plants were sampled for the fleet study. Samples of these plants' refuse streams were collected and their REE and ash contents were determined. Coal from the Eagle seam, Fire Clay seam, and Fire Clay Rider were collected and tested during the concentration phase. Samples of a waste coal from the Pittsburgh seam and a coal combustion by prodcut were also provided by a third party. The separation methods investigated include multi-gravity separation, electrostatic separation, and selective oil agglomeration. Partition curves from x-ray sorting devices were also applied to REE float-sink data as well. The results of this work show that REEs tend to partition with low ash material when viewing the results on an ash basis. Finally, the third phase of this work involved the application of x-ray sorting technology on different coals. This work showed that the x-ray sorting technology in question is capable of effectively treating prescreened feed with a size range of 2" x 1/4". The work also shows that the x-ray sorting technology also has applications in the power generation field, where it can be used to eliminate elements of environmental concern. / Ph. D.

Scanning electron microscopy based automated mineralogy (SEM-AM) is a combined analytical tool initially designed for the characterisation of ores and mineral processing products. Measurements begin with the collection of backscattered electron (BSE) images and their handling with image analysis software routines. Subsequently, energy dispersive X-ray spectra (EDS) are gained at selected points according to the BSE image adjustments. Classification of the sample EDS spectra against a list of approved reference EDS spectra completes the measurement. Different classification algorithms and four principal SEM-AM measurement routines for point counting modal analysis, particle analysis, sparse phase search and EDS spectral mapping are offered by the relevant software providers. Application of SEM-AM requires a high-quality preparation of samples. Suitable non-evaporating and electron-beam stable epoxy resin mixtures and polishing of relief-free surfaces in particles and materials with very different hardness are the main challenges. As demonstrated by case examples in this contribution, the EDS spectral mapping methods appear to have the most promising potential for novel applications in metamorphic, igneous and sedimentary petrology, ore fingerprinting, ash particle analysis, characterisation of slags, forensic sciences, archaeometry and investigations of stoneware and ceramics. SEM-AM allows the quantification of the sizes, geometries and liberation of particles with different chemical compositions within a bulk sample and without previous phase separations. In addition, a virtual filtering of bulk particle samples by application of numerous filter criteria is possible. For a complete mineral phase identification, X-ray diffraction data should accompany the EDS chemical analysis. Many of the materials which potentially could be characterised by SEM-AM consist of amorphous and glassy phases. In such cases, the generic labelling of reference EDS spectra and their subsequent target component grouping allow SEM-AM for interesting and novel studies on many kinds of solid and particulate matter which are not feasible by other analytical methods.