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Issue 5, 2011
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Quantitative HPLC-ICP-MS analysis of antimony redox speciation in complex sample matrices: new insights into the Sb-chemistry causing poor chromatographic recoveries

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Abstract

In solution antimony exists either in the pentavalent or trivalent oxidation state. As Sb(III) is more toxic than Sb(V), it is important to be able to perform a quantitative speciation analysis of Sb's oxidation state. The most commonly applied chromatographic methods used for this redox speciation analysis do, however, often show a low chromatographic Sb recovery when samples of environmental or biological origin are analysed. In this study we explored basal chemistry of antimony and found that formation of macromolecules, presumably oligomeric and polymeric Sb(V) species, is the primary cause of low chromatographic recoveries. A combination of HPLC-ICP-MS, AFFF-ICP-MS and spin-filtration was applied for analysis of model compounds and biological samples. Quantitative chromatographic Sb redox speciation analysis was possible by acidic hydrolysis of the antimony polymers prior to analysis. Sample treatment procedures were studied and the optimum solution was acidic hydrolysis by 1 M HCl in the presence of chelating ligands (EDTA, citrate), which stabilise the trivalent oxidation state of Sb.

Graphical abstract: Quantitative HPLC-ICP-MS analysis of antimony redox speciation in complex sample matrices: new insights into the Sb-chemistry causing poor chromatographic recoveries

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Publication details

The article was received on 13 Oct 2010, accepted on 22 Nov 2010 and first published on 14 Dec 2010


Article type: Paper
DOI: 10.1039/C0AN00796J
Citation: Analyst, 2011,136, 996-1002
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    Quantitative HPLC-ICP-MS analysis of antimony redox speciation in complex sample matrices: new insights into the Sb-chemistry causing poor chromatographic recoveries

    C. Hansen, B. Schmidt, E. H. Larsen, B. Gammelgaard, S. Stürup and H. R. Hansen, Analyst, 2011, 136, 996
    DOI: 10.1039/C0AN00796J

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