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Determination of Germanium Content in Coal Ash by Wavelength-Dispersive X-Ray Fluorescence Spectrometry and Inductively Coupled Plasma - Mass Spectrometry

A method for the determination of Ge in coal ash by wavelength dispersive X-ray fluorescence (WDXRF) spectrometry has been developed. Using the Compton peak for matrix correction, fused glass discs (1 part ash + 9 parts Li,B,O&iBO,), and synthetic coal ash standards, we have established a calibration line with a correlation coefficient of 0.999. This method was found to be applicable to Ge content from 10 to 12,000 ppm in coal ash. The relative standard deviation of eight aliquots of a fly ash sample was less than 2%. The accuracy of this method was evaluated by comparison with Ge content as determined by inductively coupled plasma-mass spectrometry. Relative percent differences between these two methods were less than 10%. This method can be applied to other geological materials in which Ge occurs as GeO, or can be converted to oxides after ignition. Four instrumental methods: gas chromatography, graphite finnace atomic absorption spectrometry, wavelength-dispersive X-ray fluorescence spectrometry and inductively coupled plasma-mass spectrometry, were compared for the determination of Ge. WDXRF is considered to be a convenient instrumental technique for Ge determination in coal, coal-derived materials and most geological samples. Germanium is generally enriched in the organic fraction of coal. After combustion, Ge is found to be enriched in fly ash instead of bottom ash. Among fly ash, Ge is more enriched in the fine fraction. This finding may make fly ash an economically viable resource for Ge.