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Charcoal-painted images from the French Neolithic Villevenard hypogea: an experimental protocol for radiocarbon dating of conserved and in situ carbon with consolidant contamination

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Abstract

A conserved painting removed from a Neolithic collective grave in Marne, France, provided an opportunity for radiocarbon dating to place Les Ronces Hypogeum 21 (Villevenard) into the chronology of that region. Chemical analysis with direct analysis in real time (DART) mass spectrometry, Fourier transform infrared (FTIR) spectroscopy and gas chromatography-mass spectrometry (GC-MS) of samples from the painting revealed the presence of two kinds of wax (beeswax and paraffin or microcrystalline wax) that likely were added during the conservation, a drying oil like linseed oil, as well as markers of pine resin that may arise from turpentine or colophony. A new pretreatment protocol of chloroform followed by pH 8 phosphate buffer was developed, which yielded sufficient material for plasma-chemical oxidation and AMS radiocarbon dating. The radiocarbon dates place the image from Hypogeum 21 at the more recent end of the chronology that spans from the sixth to the third millennia cal BC for the Neolithic in France.

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Acknowledgements

This research project has been possible thanks to the Spanish Ministry of Economy’s support through a research grant (HAR2015-68595-P and PGC2018-099405-B-I00) and one of us (RAA) received support from the Eastern Michigan University Provost’s Office Faculty Research Fellowship and Research Support Awards, Eastern Michigan University Chemistry Department, and Sellers Fund. The AccuTOF-DART mass spectrometer was purchased under NSF MRI-R2 award #0959621.

We would like to thank Rosa Barroso (University of Alcalá), Juan F. Ruiz (University of Castilla la Mancha), our colleagues from the Faculty of Biology from the Autónoma University of Madrid, Arturo Morales and Oscar Cambra, and our colleagues from the University of Vigo, especially Ana Villa, for their contributions to this work. RAA gives special thanks to EMU student Chelsea Van Buskirk for her help with data analysis.

Both the director and team of the Epernay Museum and the Service Régionale de l’Archeologie have kindly given us support. This research has been developed in the framework of the Saint-Gond Neolithic program.

Funding

This study received funding from the Spanish Ministry of Economy research grants HAR2015-68595-P and PGC2018-099405-B-I00 to P. Bueno Ramírez; internal funding to R.A. Armitage from Eastern Michigan University Provost’s Office Faculty Research Fellowship and Research Support Awards, Eastern Michigan University Chemistry Department, and Sellers Fund; and National Science Foundation MRI-R2 award #0959621 to Armitage for AccuTOF-DART instrumentation.

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Authors and Affiliations

  1. Department of Chemistry, Eastern Michigan University, Ypsilanti, MI, 48197, USA

    Ruth Ann Armitage & Tara Fairchild

  2. Department of Historia y Filosofía, Section Prehistory, University of Alcalá, 28880, Alcalá de Henares, Spain

    Primitiva Bueno-Ramírez & Rodrigo de Balbín-Behrmann

  3. Archaeology Earth History Society Lab, CNRS, University of Burgundy, 21000, Dijon, France

    Rémi Martineau

  4. Escola Superior de Conservación e Restauración de Bens Culturais, Universidad de Vigo, 36002, Vigo, Spain

    Fernando Carrera-Ramírez

  5. W. M. Keck Carbon Cycle Accelerator Mass Spectrometry Laboratory, Earth System Science Department, University of California, Irvine, Irvine, CA, 92697-3100, USA

    John Southon

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  1. Ruth Ann Armitage
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Correspondence to Ruth Ann Armitage.

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Armitage, R.A., Bueno-Ramírez, P., de Balbín-Behrmann, R. et al. Charcoal-painted images from the French Neolithic Villevenard hypogea: an experimental protocol for radiocarbon dating of conserved and in situ carbon with consolidant contamination. Archaeol Anthropol Sci 12, 123 (2020). https://doi.org/10.1007/s12520-020-01077-3

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