Problems with radiocarbon dating the Middle to Upper Palaeolithic transition in Italy

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Abstract

Radiocarbon dating of material from Late Pleistocene archaeological sites is challenging. Small amounts of modern 14C-labelled contamination will significantly affect the reliability of dates from the period, producing erroneous results. Recent developments in sample pre-treatment chemistry have shown that problems in reliable age determination during this period are surmountable. In this paper we provide an example of one such case, from the Middle to Upper Palaeolithic transitional site of the Grotta di Fumane, in northern Italy. We AMS dated two fractions of the same charcoal samples derived from a series of superimposed Mousterian, Aurignacian and Gravettian levels excavated at the site. One fraction was treated using the routine acid–base–acid (ABA) method, the other with the more rigorous acid–base-oxidation/stepped combustion (ABOx–SC) method. The latter method produced consistently older, and almost certainly more reliable, results. The eruption of the known-age Campanian Ignimbrite from the Phlegrean Fields near present-day Naples at 39.3 ka yr BP seals Ulluzzian and Proto Aurignacian levels in the south of Italy. Equivalent cultural levels are present at Fumane and the results obtained with the ABOx–SC methods are consistent with the ages inferred for sites in the south of Italy based on the presence of the Campanian Ignimbrite. New results from a sample found beneath the Campanian Ignimbrite at the Russian site of Kostenki, obtained using both the ABA and ABOx–SC, methods are also presented. They support the conclusion reached at Fumane by demonstrating that, in many cases, the ABOX–SC treatment effectively removes contamination where the ABA treatment does not. The results of the work offer a sobering examination of the problems inherent in the current radiocarbon database relating to the period, and highlight the dangers of an uncritical use of the corpus of 14C results obtained over the last few decades. Based on our results, we predict that more than 70% of the 53 previously available determinations from Fumane are erroneously young. A way forward is suggested, using these improved chemical preparation methods, applying analytical methods to characterise the material dated, and testing existing site chronologies to establish which previous determinations are liable to be inaccurate.

Introduction

Radiocarbon dates provide the framework for understanding the chronology of the European Middle and Upper Palaeolithic transition. Unfortunately, the method is plagued with problems in its proper application through this period because the low amount of residual radiocarbon (<3%, equivalent to ∼30,000 BP1) may be significantly influenced by the trace presence of contaminating carbon of a more recent age. The application of radiocarbon dating over almost 60 years has created a blurred vision of chronology over the latter part of the Late Pleistocene period in Europe, and this has, in turn, provided fertile ground for the strong debates that characterise the discipline (eg. D'Errico et al., 1998, Mellars, 1999, Zilhão and D'Errico, 1999). Several thousand radiocarbon determinations are available on various databases2. However, deciphering quite which of them are reliable and which not, is an often impossible task, because the key information we require in order to diagnose this, such as a pre-treatment method description and basic analytical data, is almost always unavailable. Recent developments have signalled that an improvement in the situation is near. A new interim calibration curve reaching ∼55,000 BP is due to be released soon through the INTCAL group and more refined pre-treatment methods are being applied which, along with improved instrumentation, are facilitating increased levels of accuracy. However, much more work remains to be done. In this paper we point to the crucial requirements of sample preparation and chemistry in deriving reliable radiocarbon dates and provide a case study from the Italian Palaeolithic that illustrates the pitfalls and problems apparent.

Section snippets

The chronology of the Italian Palaeolithic during Marine Isotope Stage (MIS) 3

Several authors (Mussi, 2001, Giaccio et al., 2006, Peresani, 2006, Bietti and Negrino, 2007, Milliken, 2007) have recently reviewed the Italian Middle to Upper Palaeolithic sequence, a period which saw the disappearance of Mousterian and Uluzzian techno-complexes, considered as an expression of the last Neanderthals, and the appearance of the Aurignacian (or the Proto Aurignacian, in its earliest manifestation3

Charcoal dating

Charcoal is usually assumed to be a reliable material for dating, if the archaeological context is secure and inbuilt age issues can be set to one side. Routine treatment of such material in radiocarbon laboratories usually comprises an acid–base–acid (ABA) sequence. This pre-treatment method is designed to remove carbonates and humic complexes using acidic and basic solutions respectively (the latter most commonly using NaOH), with any atmospheric carbon dioxide adsorbed during the base wash

The site of Grotta di Fumane

In recent work we have been re-evaluating the radiocarbon corpus from a key site in northern Italy, the Grotta di Fumane. The site lies at 350 m above sea level at the southern fringe of the Venetian Pre-Alps (Fig. 1) and is part of a complex karst system made up of several cavities which together form a sedimentary succession over 10 m thick (Fig. 2). It has produced a dated sequence for the Middle to Upper Palaeolithic which spans the period from MIS 5–MIS2 (Peresani et al., 2008). This has

Materials and methods

The Fumane radiocarbon sequence was re-examined to determine whether some of the ages previously obtained were reliable or not. Several charcoal samples were dated using both ABOx–SC and ABA techniques, and the results were compared with previous measurements from throughout the sequence. Consistent results between ABOx–SC and ABA determinations would suggest strongly that the original chronometric sequence was reproducible, though extremely variable in radiocarbon age. This result would

Results

We can compare our new results with the series listed in Cremaschi et al., 2005, Giaccio et al., 2006 and Peresani et al. (2008)(see Table 1 above). The results for Level A2 in Table 3, (OxA-11360, an ABA determination, for example, may be compared with OxA-17570, an ABOx–SC determination; and OxA-11347 (ABA) with OxA-17569 (ABOx–SC)) show clearly that routine ABA pre-treatment was not sufficient to remove contamination from charcoal excavated within this context. The substantially older

Discussion

A revised chronology for the Middle to Upper Palaeolithic sequence at Fumane is shown in Fig. 3 using a modelled Bayesian sequence generated with OxCal 4.0 (Bronk Ramsey, 2001). In the model we have compared (see discussion in van der Plicht et al., 2004) our ABOx–SC radiocarbon determinations against the Cariaco Basin 14C record published by Hughen et al. (2006). This dataset has a greater number of radiocarbon analyses than the previously published data (Hughen et al., 2004), and an age model

Conclusions

Our new ABOx–SC series shows that the previous chronology from the important site of the Grotta di Fumane is dominated by radiocarbon measurements that are erroneously young, but they also show that there are some samples of charcoal, mostly <30 ka BP, which appear to be less contaminated than others and which produce statistically identical results regardless of pre-treatment chemistry. This mirrors results from other sites in Malaysia, Europe and the Palaeolithic of the Mediterranean (Higham

Acknowledgements

The radiocarbon determinations were funded by a grant to FB and TH from the NERC-AHRC Oxford Radiocarbon Accelerator Dating Service (ORADS). Research at Fumane is managed by the Ferrara and Milano I Universities in the framework of a project supported by the Soprintendenza per i Beni Archeologici del Veneto, Cariverona Foundation, Comunità Montana della Lessinia, Comune di Fumane. We are grateful to the staff of the ORAU. Ms R. Wood is funded by a tied-NERC studentship (grant NE/D014077/1). Ms

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