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The Crystalline State of Archaeological Bone Material

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Across the Alps in Prehistory

Abstract

Isotope studies on archaeological bone mineral require a validation of the investigated sample material. Diagenetic alteration or contaminated bone mineral should be recognized as such and not be used for conclusions requiring pristine material. X-ray diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR) provide two complementary tools to characterize the state of the bone mineral. While IR measurements are easy and rapid, their interpretation is still largely empirical. Modern XRD analysis is more demanding with respect to experiment and data evaluation, but it is based on rigorous theoretical modelling of the observed data. Our study involved both uncremated animal bone samples from the alpine region covering ages from 7600 to 550 years before present, as well as cremated human bone remains in comparison with experimentally cremated bovine bone. All samples were mechanically cleaned to remove soil, and inner and outer periosteal surfaces were mechanically removed. We avoided visually decomposed bones completely. The mineralogic state of the thus cleaned, uncremated samples showed only minor systematic changes with archaeologic age. The changes are most pronounced for the lattice parameter and crystalline domain size in the short dimension of the original bone-apatite platelets. The long direction corresponding to the crystallographic c-axis of the apatite appears almost unaffected. We conclude that in the investigated samples, there is only a minor diagenetic alteration of the original bone mineral, possibly related to exchange of carbonate by hydroxyl or fluorine.

From annealing experiments with bovine femur bone material at different temperatures for 1 h annealing time, we established calibration curves to be used to estimate cremation temperatures of bones based on FTIR spectra and X-ray diffractograms. While the evaluation of the diffractograms is rigorously based on a physical model, the evaluation of spectral components in FTIR spectra is empirical. The experiments indicate that original bone apatite contains little–if any–OH− such that it is carbonate-H2O-apatite (rather than hydroxyapatite), and with increasing temperature, water and carbonate leave the material, and from 600 °C, hydroxyapatite is formed with increasing purity and crystallite size with increasing temperature. The analysis of some cremated bones from Urnfield Culture sites of Eching and Zuchering, southern Bavaria, clearly indicated that the archaeological cremated bones are inhomogeneous materials where different parts of the samples were subjected to different cremation temperatures and/or times at temperature within fractions of centimetres. This can be attributed to the conditions in the pile of burning logs and burning tissue. Nevertheless, a fair estimation of cremation temperatures is certainly possible even where the FTIR approach and the XRD approach still do not have a full mutual consistency. Future work needs to address the anatomical variability of original bone material within and between species in much more detail than is known at present. Beyond the well-defined temperature/time conditions in furnace annealing experiments, cremation experiments with bone material analyses must also be done in more realistic conditions as they occur in a funeral pyre.

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Acknowledgement

We thank the Deutsche Forschungsgemeinschaft, DFG, for financial support in Forschergruppe FOR1670, projects SCHM930/12-1 and GR959/21-1 and 20-1.

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Authors and Affiliations

  1. Sektion Kristallographie, Ludwig-Maximilians-Universität, Munich, Germany

    Wolfgang W. Schmahl & Balazs Kocsis

  2. Biozentrum, Ludwig-Maximilians-Universität, Martinsried, Germany

    Anita Toncala, Dominika Wycisk & Gisela Grupe

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  1. Wolfgang W. Schmahl
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Correspondence to Wolfgang W. Schmahl .

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  1. LMU München Biozentrum Martinsried, Martinsried, Bayern, Germany

    Gisela Grupe

  2. Staatssammlung f. Anthropologie und Paläoanatomie, München, Bayern, Germany

    Andrea Grigat

  3. LMU München Biozentrum Martinsried, Martinsried, Bayern, Germany

    George C. McGlynn

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Schmahl, W.W., Kocsis, B., Toncala, A., Wycisk, D., Grupe, G. (2017). The Crystalline State of Archaeological Bone Material. In: Grupe, G., Grigat, A., McGlynn, G. (eds) Across the Alps in Prehistory. Springer, Cham. https://doi.org/10.1007/978-3-319-41550-5_4

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