Abstract
For the evaluation of the speciation of Sn in solid samples, a leaching sequence is presented, which takes into account the special properties of the element investigated. The sample is leached with ethanol (organics), 25% acetic acid (carbonates), oxalate (coprecipitation upon Fe/Mn-hydroxides), then oxidized with KMnO4 (sulfides), and finally sublimed with NH4I (cassiterite); the silicate fraction is found as the difference to the total decomposition value (e.g. LiBO2).
Final determinations are done by hydride AAS from tartaric acid-solutions, except the ethanol fraction which is submitted to ETA-AAS. In the furnace, addition of HNO3 and H2O2 and rapid heating in the gas-stop mode results in equal sensitivity of organic and inorganic tin in the ethanol extract. The proposed method is checked by coprecipitation/adsorption experiments and by addition of tin-bearing minerals to a natural sediment.
The method was applied to fresh water sediments. In sediment cores, the KMnO4 fraction was dominant, whereas in an oxic surface sediment NH4I releases the main fraction (cassiterite).
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Sager, M. Speciation of tin in sediments and soils by leaching. Mikrochim Acta 90, 129–139 (1986). https://doi.org/10.1007/BF01364295
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DOI: https://doi.org/10.1007/BF01364295