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Direct μ-flow injection isotope dilution ICP-MS for the determination of heavy metals in oil samples

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Abstract

The determination of trace elements in oil samples and their products is of high interest as their presence significantly affects refinery processes and the environment by possible impact of their combustion products. In this context, inductively coupled plasma mass spectrometry (ICP-MS) plays an important role due to its outstanding analytical properties in the quantification of trace elements. In this work, we present the accurate and precise determination of selected heavy metals in oil samples by making use of the combination of μ-flow direct injection and isotope dilution ICP-MS (ICP-IDMS). Spike solutions of 62Ni, 97Mo, 117Sn and 206Pb were prepared in an organic solvent, mixed directly with the diluted oil samples and tested to be fit for purpose for the intended ID approach. The analysis of real samples revealed strong matrix effects affecting the ICP-MS sensitivity, but not the isotope ratio measurements, so that accurate results are obtained by ICP-IDMS. Typical relative standard deviations were about 15% for peak area and peak height measurements, whereas the isotope ratios were not significantly affected (RSD < 2%). The developed method was validated by the analysis of a metallo-organic multi-element standard (SCP-21, typically applied as a calibration standard) and the standard reference material SRM1084a (wear metals in lubricating oil). The obtained results were in excellent agreement with the certified values (recoveries between 98% and 102%), so the proposed methodology of combining μ-flow direct injection and ICP-IDMS can be regarded as a new tool for the matrix-independent, multi-element and reliable determination of trace elements in oil and related organic liquids.

Determination of heavy metals in oil samples by ICP-IDMS

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Acknowledgements

The authors thank Thermo Fisher Scientific, Bremen, Germany, and Merck KGaA, Darmstadt, Germany, for providing us the instrumentation. J. Bettmer and D.J. Kutscher acknowledge the Spanish Ministry for Science and Innovation (MICINN) for the contracts within the Ramón y Cajal and the FPU programme, respectively, and the support within the project CTQ2008-01725.

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Authors and Affiliations

  1. Department of Physical and Analytical Chemistry, Faculty of Chemistry, University of Oviedo, C/Julián Clavería 8, 33006, Oviedo, Spain

    Jörg Bettmer, Daniel J. Kutscher & Alfredo Sanz-Medel

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

    Jens Heilmann & Klaus G. Heumann

Authors
  1. Jörg Bettmer
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  2. Jens Heilmann
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  3. Daniel J. Kutscher
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  4. Alfredo Sanz-Medel
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  5. Klaus G. Heumann
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Corresponding authors

Correspondence to Jörg Bettmer or Klaus G. Heumann.

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Published in the 10th Anniversary Issue.

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Bettmer, J., Heilmann, J., Kutscher, D.J. et al. Direct μ-flow injection isotope dilution ICP-MS for the determination of heavy metals in oil samples. Anal Bioanal Chem 402, 269–275 (2012). https://doi.org/10.1007/s00216-011-5420-6

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  • DOI: https://doi.org/10.1007/s00216-011-5420-6

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