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Development of an accurate, sensitive, and robust isotope dilution laser ablation ICP-MS method for simultaneous multi-element analysis (chlorine, sulfur, and heavy metals) in coal samples

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Abstract

A method for the direct multi-element determination of Cl, S, Hg, Pb, Cd, U, Br, Cr, Cu, Fe, and Zn in powdered coal samples has been developed by applying inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with laser-assisted introduction into the plasma. A sector-field ICP-MS with a mass resolution of 4,000 and a high-ablation rate laser ablation system provided significantly better sensitivity, detection limits, and accuracy compared to a conventional laser ablation system coupled with a quadrupole ICP-MS. The sensitivity ranges from about 590 cps for 35Cl+ to more than 6 × 105 cps for 238U+ for 1 μg of trace element per gram of coal sample. Detection limits vary from 450 ng g−1 for chlorine and 18 ng g−1 for sulfur to 9.5 pg g−1 for mercury and 0.3 pg g−1 for uranium. Analyses of minor and trace elements in four certified reference materials (BCR-180 Gas Coal, BCR-331 Steam Coal, SRM 1632c Trace Elements in Coal, SRM 1635 Trace Elements in Coal) yielded good agreement of usually not more than 5% deviation from the certified values and precisions of less than 10% relative standard deviation for most elements. Higher relative standard deviations were found for particular elements such as Hg and Cd caused by inhomogeneities due to associations of these elements within micro-inclusions in coal which was demonstrated for Hg in SRM 1635, SRM 1632c, and another standard reference material (SRM 2682b, Sulfur and Mercury in Coal). The developed LA-ICP-IDMS method with its simple sample pretreatment opens the possibility for accurate, fast, and highly sensitive determinations of environmentally critical contaminants in coal as well as of trace impurities in similar sample materials like graphite powder and activated charcoal on a routine basis.

LA-ICP-IDMS allows direct multi-element determination in powdered coal samples

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Acknowledgement

The authors are grateful to the Stiftung Rheinland-Pfalz für Innovation for financial support. S.B. and T.P. also acknowledge support by the Austrian Science Fund FWF (START project 267-N11).

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Authors and Affiliations

  1. Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, University of Natural Resources and Applied Life Sciences, Muthgasse 18, 1190, Vienna, Austria

    Sergei F. Boulyga & Thomas Prohaska

  2. Institute of Inorganic Chemistry and Analytical Chemistry, Johannes Gutenberg-University, Duesbergweg 10–14, 55099, Mainz, Germany

    Sergei F. Boulyga, Jens Heilmann & Klaus G. Heumann

Authors
  1. Sergei F. Boulyga
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  2. Jens Heilmann
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  3. Thomas Prohaska
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  4. Klaus G. Heumann
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Correspondence to Sergei F. Boulyga.

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Boulyga, S.F., Heilmann, J., Prohaska, T. et al. Development of an accurate, sensitive, and robust isotope dilution laser ablation ICP-MS method for simultaneous multi-element analysis (chlorine, sulfur, and heavy metals) in coal samples. Anal Bioanal Chem 389, 697–706 (2007). https://doi.org/10.1007/s00216-007-1485-7

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  • DOI: https://doi.org/10.1007/s00216-007-1485-7

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