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Improved AMS 14C Dating of Shell Carbonates Using High-Precision X-Ray Diffraction and a Novel Density Separation Protocol (Cards)

Published online by Cambridge University Press:  18 July 2016

Katerina Douka ,
Robert E M Hedges  and
Thomas F G Higham
Katerina Douka*
Affiliation:
Research Laboratory for Archaeology and the History of Art, University of Oxford, Dyson Perrins Building, South Parks Road, Oxford OX1 3QY, United Kingdom Oxford Radiocarbon Accelerator Unit, Research Laboratory for Archaeology and the History of Art, University of Oxford, Dyson Perrins Building, South Parks Road, Oxford OX1 3QY, United Kingdom
Robert E M Hedges
Affiliation:
Research Laboratory for Archaeology and the History of Art, University of Oxford, Dyson Perrins Building, South Parks Road, Oxford OX1 3QY, United Kingdom
Thomas F G Higham
Affiliation:
Oxford Radiocarbon Accelerator Unit, Research Laboratory for Archaeology and the History of Art, University of Oxford, Dyson Perrins Building, South Parks Road, Oxford OX1 3QY, United Kingdom
*
Corresponding author. Email: katerina.douka@rlaha.ox.ac.uk
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Abstract

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One critical variable in the successful application of radiocarbon dating is the effective removal of carbonaceous contaminants. In the case of marine carbonates, contamination appears usually in the form of secondary low-magnesium calcite, the stable polymorph of calcium carbonate and byproduct of the post-mortem recrystallization or replacement of the autochthonous phase, originally in the form of high-magnesium calcite or aragonite. Depending on the nature of the depositional environment, the secondary phase may be contemporary in age with the original shell carbonate and may have even been derived from it by dissolution-recrystallization processes, or can be an exogenous contaminant of younger or older age. The limited ability of current pretreatment protocols to detect and remove the secondary mineralogical phases prior to dating carbonates has been one of the reasons marine shell and coral 14C determinations are often difficult to validate in terms of their reliability. We have developed a new pretreatment protocol designed to achieve greater reliability and accuracy in the dating of this material. The method entails 2 steps. The first one involves the improved detection and quantification of secondary calcite in aragonite using X-ray diffraction, at a precision of ∼0.1% and ∼0.8%, respectively. Next, where this is required, a novel density separation step using non-toxic heavy liquids (CarDS) is applied to the diagenetic sample. This enables the clear separation of calcite and aragonite, with only the latter kept for dating. We have applied the new steps, screening and separation, on standard and archaeological examples and our initial results suggest that it is successful and reproducible. In this paper, we describe the method and initial results.

Type
Methods, Applications, and Developments
Information
Radiocarbon , Volume 52 , Issue 2: 20th Int. Radiocarbon Conference Proceedings , 2010 , pp. 735 - 751
Copyright
Copyright © 2010 by the Arizona Board of Regents on behalf of the University of Arizona 

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