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ICP-MS DETERMINATION OF 45 TRACE ELEMENTS IN WHOLE COAL USING MICROWAVE OVEN ACID DIGESTION FOR SAMPLE PREPARATION
Authors:Sandro FADDA  Alessandro RIVOLDINI  Ignazio CAU
Institution:C.N.R. Centro Studi Geominerari e Mineralurgici, Piazza D'Armi 09100 Cagliari, Italy;Istituto di Giacimenti Minerari, Piazza D'Armi 09100 Cagliari, Italy;Ecosystems, Laboratorio Privato di Analisi e Ricerca Applicata, via F.lli Vivaldi N°7 Porto Torres (SS), Italy
Abstract:The microwave oven acid digestion technique has been routinely applied to the ICP-MS multielement analysis of whole powdered coal. Samples were treated with a mixture of HF/aqua regia/HClO4 in closed Teflon PFA vessels without any pre-treatment. Complete dissolution of the coal matrix is not required, but only one that results in quantitative and reproducible recovery of more than 40 trace elements with minimum digestion time, minimum use of reagents and minimal operator attendance. The precision of the analysis as well as the repeatability of the sample preparation procedure and precision of instrumental measurements have been evaluated. Eight coal standards, including NBS SRM 1632b, 3 South Africa Reference Materials (SARMs) 18 to 20 and 4 USA ARs 1800 to 1803 were analysed in this manner providing data for all the 14 rare earth elements along with others of geochemical interest, technological relevance as well as environmental and health concern. The results, from the ppb level to several ppm, are discussed for all the elements including detection and quantification limits, precision and accuracy. In general, good agreement was achieved with the certified and/or available published values.
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