Accurate compound-specific 14C dating of archaeological pottery vessels

Abstract

Pottery is one of the most commonly recovered artefacts from archaeological sites. Despite more than a century of relative dating based on typology and seriation1, accurate dating of pottery using the radiocarbon dating method has proven extremely challenging owing to the limited survival of organic temper and unreliability of visible residues2,3,4. Here we report a method to directly date archaeological pottery based on accelerator mass spectrometry analysis of 14C in absorbed food residues using palmitic (C16:0) and stearic (C18:0) fatty acids purified by preparative gas chromatography5,6,7,8. We present accurate compound-specific radiocarbon determinations of lipids extracted from pottery vessels, which were rigorously evaluated by comparison with dendrochronological dates9,10 and inclusion in site and regional chronologies that contained previously determined radiocarbon dates on other materials11,12,13,14,15. Notably, the compound-specific dates from each of the C16:0 and C18:0 fatty acids in pottery vessels provide an internal quality control of the results6 and are entirely compatible with dates for other commonly dated materials. Accurate radiocarbon dating of pottery vessels can reveal: (1) the period of use of pottery; (2) the antiquity of organic residues, including when specific foodstuffs were exploited; (3) the chronology of sites in the absence of traditionally datable materials; and (4) direct verification of pottery typochronologies. Here we used the method to date the exploitation of dairy and carcass products in Neolithic vessels from Britain, Anatolia, central and western Europe, and Saharan Africa.

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Fig. 1: Site location map, partial gas chromatograms and stable isotope determination of compound-specific radiocarbon-dated lipid residues preserved in Neolithic pottery vessels.
Fig. 2: Sweet Track timbers, a pottery vessel and calibrated radiocarbon dates.
Fig. 3: Drawings, correspondence analysis and radiocarbon dates of Neolithic vessels from Alsace (France) modelled using Bayesian statistics.

Data availability

All data generated during this study are included in the Article, Extended Data Figs. 19, Extended Data Table 1 and Supplementary Information.

Code availability

The codes used in OxCal for statistical modelling are provided in the Supplementary Information.

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Acknowledgements

We thank the European Research Council for funding an advanced grant (NeoMilk, FP7-IDEAS-ERC/324202) and a proof-of-concept grant (LipDat, H2020 ERC-2018-PoC/812917) to R.P.E., financing a PhD to E. Casanova and postdoctoral contract to M.R.-S. and J.S., and a postdoctoral contract to E. Casanova; the BRAMS facility for the radiocarbon measurements, establishment of which was jointly funded by the NERC, BBSRC and University of Bristol; P. Monaghan for his help with the radiocarbon sample preparation; the Polish National Science Centre (decision DEC-2012/06/M/H3/00286) for financing the work in the upper levels at Çatalhöyük; the Department of Antiquities in Tripoli, Libya for permits and Sapienza University of Rome and Italian Ministry of Foreign Affairs for funding the fieldwork in Libya; MOLA (Museum of London Archaeology) for excavating and providing potsherds from Principal Place (PPL11), London EC2/E1; and B. Schnitzler from the Palais Rohan for accessing the material from Rosheim, A. Mulot from the Achéologie Alsace (Centre of Conservation and Study) for accessing the material from Ensisheim, R. W. Schmitz from the LVR-Landes Museum Bonn for accessing the material from Königshoven 14 and R. Brunning from the South West Heritage Trust for sharing excavation photographs of the Sweet Track.

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Authors

Contributions

R.P.E. conceived the project. E. Casanova, R.P.E. and A. Bayliss wrote the paper. E. Casanova, T.D.J.K. and R.P.E. developed the method for dating lipids. E. Casanova, J.D. and T.G. performed the preparation of pottery vessels for radiocarbon analysis. E. Casanova and T.D.J.K. generated the radiocarbon measurements and performed data analysis. A. Bayliss undertook the statistical modelling of the radiocarbon dates. M.Z.B. advised on the stratigraphic sequence of the TP area of Çatalhöyük East. A.M. performed the stratigraphic analysis of the TP area of Çatalhöyük East and chronological analysis of the LBK from the Polish lowlands and M.K. helped with the selection and provided the pottery vessels from these sites. C.J. and P.L. excavated the Alsatian sites. A. Denaire and P.L. performed the correspondence analysis of the Alsace region. S.d.L. advised on the stratigraphic sequence and pottery analysis of Takarkori and R.R. studied the pottery assemblage. E. Casanova, M.R.-S. and J.S. sampled the LBK sites. M.R.-S. coordinated and processed the analyses of sherds from the LBK culture and from Çatalhöyük East. A. Barclay advised on project design. B.C directed excavations of the Sweet Track and S.M. provided the pottery vessels. E. Claßen analysed the material and advised sampling for Königshoven 14. M.I. excavated and provided vessels from Cuiry-lès-Chaudardes. I.v.W. excavated and advised sampling from The Netherlands and P.v.d.V. analysed the material. A. Daykin excavated the site of Principal Place, London EC2/E1 as project manager and J.C. studied the pottery material.

Corresponding author

Correspondence to Richard P. Evershed.

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Competing interests

The authors declare no competing interests.

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Peer review information Nature thanks Graeme Barker and the other, anonymous, reviewer(s) for their contribution to the peer review of this work.

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Extended data figures and tables

Extended Data Fig. 1 Schematic showing the stratigraphic information of the Neolithic occupation of the TP area at Çatalhöyük (Turkey).

This information was included in the chronological model defined in Extended Data Fig. 2. Contexts containing potsherds dated in this study are highlighted in green.

Extended Data Fig. 2 Probability distributions of dates from Neolithic deposits in the TP area at Çatalhöyük, Turkey.

Data include the results on absorbed fatty acids in pottery sherds listed in Extended Data Table 1. Each distribution represents the relative probability that an event occurs at a particular time. For each date, two distributions are plotted: one in outline, which is the result of a simple radiocarbon calibration, and a solid one, based on the chronological model used. The distributions in green correspond to the potsherds, distributions in black show the pre-existing chronology. Distributions other than those relating to particular samples correspond to aspects of the model. For example, the distribution ‘end East Mound occupation’ is the estimated date at which the Neolithic occupation of the East Mound ended at Çatalhöyük. Measurements followed by a question mark and shown in outline have been excluded from the model for reasons described in table 1 of a previous study11 and are simple calibrated dates34. The large square brackets down the left side, along with the OxCal keywords, define the overall model exactly.

Extended Data Fig. 3 Probability distributions of radiocarbon dates from absorbed fatty acids in LBK ceramics.

Data on absorbed fatty acids are listed in Extended Data Table 1. Black, dairy; blue, ruminant adipose; red, non-ruminant adipose. Data are shown as described for Extended Data Fig. 2.

Extended Data Fig. 4 Sensitivity analyses of radiocarbon dates on LBK ceramics.

Key parameters for the start of the use of LBK ceramics (blue distribution)—derived from the models defined in Extended Data Fig. 3, figure 8 of a previous study12, and figures 18, 19 (model 1), 20, 21 (model 2) and 22, 23 (model 3) of a previous publication13—were compared with the start of LBK lipids presented in Extended Data Fig. 3 (red distributions), and subsequently deliberately biased by 1σ, 2σ, 3σ, 4σ and 8σ to younger (orange distributions) and older (pink distributions) values. Some distributions may have been truncated.

Extended Data Fig. 5 The Tadrart Acacus Mountains in southwest Libya.

ab, The Wadi Takarkori area (dashed rectangle). c, Schematic plan of the excavated areas. All sampled sherds come from the main sector.

Extended Data Fig. 6 Site stratigraphy, photographs of potsherds and radiocarbon dates of Middle Pastoral pottery vessels from Takarkori (Libya) modelled using Bayesian statistics.

a, Stratigraphic context of sampled potsherds from Takarkori east–west profile of the southern wall of the Takarkori north–south (Extended Data Fig. 5). (a) aeolian sand; (b) sand rich in organic matter; (c) lenses of undecomposed plant remains; (d) ash; (e) charcoal; (f) slurry deposit; (g) eroded sand from the wall; (h) bedrock. b, Photographs of the five potsherds analysed showing typical Middle Pastoral decorative patterns. c, Example of temporally and spatially wide deposit of organic sands (detail of layer 25, Takarkori main sector). d, Statistical model of the Middle Pastoral period showing the comparison of pot lipid dates (in green) with previous radiocarbon measurements. Data are shown as described for Extended Data Fig. 2.

Extended Data Fig. 7 Sensitivity analyses of radiocarbon dates on vessels from Takarkori rock shelter, Libya.

Probability distributions for the beginning and end Middle Pastoral period ceramics from Takarkori rock shelter, Libya (no pot lipid dates) compared with those of the model shown in the Extended Data Fig. 6d and models including fatty acid dates that were deliberately biased by 1σ, 2σ, 4σ, 8σ, 20σ and 40σ. Data are shown as described for Extended Data Fig. 4.

Extended Data Fig. 8 Probability distributions of dates associated with the use of early Neolithic Plain Bowl pottery in southern Britain.

Prior distributions have been taken from the models described in the text and in the Supplementary Information. Data are shown as described for Extended Data Fig. 2.

Extended Data Fig. 9 Sensitivity analyses of radiocarbon dates on vessels from Principal Place, London.

Probability distributions of the start and end of early Neolithic Plain Bowl pottery in southern Britain compared with those of the model shown in Extended Data Fig. 8 and models including fatty acid dates that were deliberately biased by 2σ, 4σ, 8σ and 16σ. Data are shown as described for Extended Data Fig. 4.

Extended Data Table 1 Summary of radiocarbon dates of lipids preserved in pottery vessels

Supplementary information

Supplementary Information

This file contains the details on the methods employed (SI 1) as well as the discussion of the results for every case study presented in the paper (SI 2-7) and conclusions of the analyses (SI 8).

Reporting Summary

Supplementary Data

Sorted Table. This file contains the matrix of the correspondence analysis based on decorative motifs of main and secondary motifs during the Middle Neolithic in Alsace (SI 4).

Supplementary Data

Sweet Track OxCal Model (OXCAL file). This file is the OxCal code used for evaluation of the accurate dating of pottery vessels associated with the Sweet Track, Somerset levels, UK (SI 2).

Supplementary Data

TP OxCal Model (OXCAL file). This file is the OxCal code used for evaluation of the accurate dating of pottery vessels from the TP area at Çatalhöyük East, Turkey (SI 3).

Supplementary Data

Alsace Middle Neolithic OxCal Model (OXCAL file). This file is the OxCal code used for evaluation of the accurate dating of pottery vessels from the Alsatian Middle Neolithic, France (SI 4).

Supplementary Data

LBK lipids OxCal Model (OXCAL file). This file is the OxCal code used for evaluation of the accurate dating of pottery vessels from the LBK sites in Central Europe (SI 5).

Supplementary Data

Takarkori Middle Pastoral OxCal Model (OXCAL file). This file is the OxCal code used for evaluation of the accurate dating of pottery vessels from the Middle Pastoral period at Takarkori, Libya (SI 6).

Supplementary Data

Plain Bowl OxCal Model (OXCAL file). This file is the OxCal code used for evaluation of the accurate dating of pottery vessels from Principal Place, London, UK (SI 7).

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Casanova, E., Knowles, T.D.J., Bayliss, A. et al. Accurate compound-specific 14C dating of archaeological pottery vessels. Nature 580, 506–510 (2020). https://doi.org/10.1038/s41586-020-2178-z

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