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A modified lead–matrix separation procedure shown for lead isotope analysis in Trojan silver artefacts as an example

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Abstract

A modified Pb–matrix separation procedure using NH4HCO3 solution as eluent has been developed and validated for determination of Pb isotope amount ratios by thermal ionization mass spectrometry. The procedure is based on chromatographic separation using the Pb·Spec resin and an in-house-prepared NH4HCO3 solution serving as eluent. The advantages of this eluent are low Pb blanks (<40 pg mL−1) and the property that NH4HCO3 can be easily removed by use of a heating step (>60 °C). Pb recovery is >95 % for water samples. For archaeological silver samples, however, the Pb recovery is reduced to approximately 50 %, but causes no bias in the determination of Pb isotope amount ratios. The validated procedure was used to determine lead isotope amount ratios in Trojan silver artefacts with expanded uncertainties (k = 2) <0.09 %.

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Acknowledgments

The authors expressly thank the “Museum für Vor- und Frühgeschichte, Staatliche Museen zu Berlin”, Berlin, in particular Hermann Born and Matthias Wemhoff, for providing the samples.

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Authors and Affiliations

  1. BAM Federal Institute for Materials Research and Testing, Unter den Eichen 87, 12205, Berlin, Germany

    Jochen Vogl, Maren Koenig & Wolfgang Pritzkow

  2. PAZ Laboratorien für Archäometrie, 55543, Bad Kreuznach, Germany

    Boaz Paz

Authors
  1. Jochen Vogl
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  2. Boaz Paz
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  3. Maren Koenig
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  4. Wolfgang Pritzkow
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Corresponding author

Correspondence to Jochen Vogl.

Additional information

Published in the topical collection Isotope Ratio Measurements: New Developments and Applications with guest editors Klaus G. Heumann and Torsten C. Schmidt.

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Vogl, J., Paz, B., Koenig, M. et al. A modified lead–matrix separation procedure shown for lead isotope analysis in Trojan silver artefacts as an example. Anal Bioanal Chem 405, 2995–3000 (2013). https://doi.org/10.1007/s00216-012-6323-x

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  • DOI: https://doi.org/10.1007/s00216-012-6323-x

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