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the Tisza and Szamos rivers located in eastern Hungary are frequently polluted mostly due to mining activities in the catchment area The speciation of heavy metals is necessary for estimating the environmental mobility and bioavailability of these elements Below, the capability of TW-EPMA for the heavy metal speciation in sediment particles is demonstrated In March 2000, just a month after the world-widely discussed catastrophic cyanide pollution event, a thousand tons of heavy-metal containing sludge reached the surviving part of the Tisza River due to a tailings dam failure at Baia Borsa, Romania Sediment samples were collected from the main riverbed of the Hungarian section of Tisza at six sites, a week after the pollution event.

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All of the collected samples were subjected to bulk XRF prior to the TW-EPMA measurements, and this technique showed that some of the samples collected at the river section between 200 220 km from the pollution site, contained Cu, Zn and Pb at elevated concentrations The observed concentrations were an order of magnitude higher than the background level for river and lake sediments in Hungary (Szal ki et al, 1999; Weisz o et al, 2000) The average population of particles in the sediment samples was investigated using single-particle TW-EPMA, on samples prepared on silver foil using the inverse BSE contrast As the determination of carbon and oxygen is feasible with this method, the most abundant particle type connected with the mine pollution could be clearly identi ed as pyrite.

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Internally mixed particles consisting of aluminosilicates (natural constituents of sediment) and pyrite, zinc sul de and lead oxide were also detected The abundance of the pollution particles was below 10 % by number for the most polluted samples In order to exclusively investigate the heavy-metal containing particles, one sediment sample showing the highest pollution was prepared on silicon wafer for further analysis Using the normal BSE contrast, only particles having signi cantly higher average atomic number than that of silicon were selected for automatic measurement Although a 10 keV electron excitation energy was used, heavy metals could be identi ed and determined using L and M X-ray lines Using this measurement setup, pyrite, zinc.

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