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Combined non-destructive XRF and SR-XAS study of archaeological artefacts

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Abstract

We report on a non-destructive study of Sicilian ceramic fragments of cultural heritage interest, classified as “proto-majolica” pottery and dating back to the twelfth to thirteen centuries AD. The analytical approach used is based on the employment of two totally non-invasive spectroscopic techniques: X-ray fluorescence (XRF), using a portable energy-dispersive XRF analyser, and X-ray absorption spectroscopy, using synchrotron radiation as a probe (SR-XAS). XRF measurements allowed us to collect elemental and spatially resolved information on major and minor constituents of the decorated coating of archaeological pottery fragments, so providing preliminary results on the main components characterizing the surface. In particular, we assigned to Fe and Mn the role of key elements of the colouring agent. With the aim of obtaining more detailed information, we performed SR-XAS measurements at the Fe and Mn K-edges at the Italian BM08 beamline at the European Synchrotron Radiation Facility (Grenoble, France). The experimental data were analysed by applying principal component analysis and least-squares fitting to the near-edge part of the spectra (X-ray absorption near-edge structure) to determine the samples’ speciation. From the overall results, umber, a class of brownish pigments characterized by a mixture of hydrated iron and manganese oxides, has been ascribed as a pigmenting agent.

Fe K-edge XANES spectra of selected proto-majolica samples and reference compounds (FeO, Fe3O4, Fe2O3, Fe+SiO2). D pigmented, L not pigmented.

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Acknowledgements

The research was supported by Ministero dell’Università e della Ricerca Scientifica e Tecnologica grant MURST-PRIN2007. The authors are grateful to ESRF (Grenoble, France) for providing beam time and technical assistance.

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Authors and Affiliations

  1. I.F.M. Chemistry Department, University of Turin, Via P. Giuri, 7, 10125, Turin, Italy

    Fabrizio Bardelli

  2. Geological Science Department, University of Catania, Corso Italia 55, 95129, Catania, Italy

    Germana Barone & Paolo Mazzoleni

  3. Physics Department, University of Messina, V.le F. Stagno D’Alcontres 31, 98166, Messina, Italy

    Vincenza Crupi, Francesca Longo, Domenico Majolino & Valentina Venuti

Authors
  1. Fabrizio Bardelli
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  2. Germana Barone
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  3. Vincenza Crupi
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  4. Francesca Longo
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  5. Domenico Majolino
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  6. Paolo Mazzoleni
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  7. Valentina Venuti
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Corresponding author

Correspondence to Francesca Longo.

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Published in the special issue Analytical Chemistry for Cultural Heritage with Guest Editors Rocco Mazzeo, Silvia Prati, and Aldo Roda.

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Bardelli, F., Barone, G., Crupi, V. et al. Combined non-destructive XRF and SR-XAS study of archaeological artefacts. Anal Bioanal Chem 399, 3147–3153 (2011). https://doi.org/10.1007/s00216-011-4718-8

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  • DOI: https://doi.org/10.1007/s00216-011-4718-8

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