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Direct Radiocarbon Dating of Prehistoric Cave Paintings by Accelerator Mass Spectrometry

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Direct Radiocarbon Dating of Prehistoric Cave Paintings by Accelerator Mass Spectrometry INSTITUTE OF PHYSICS PUBLISHING MEASUREMENT SCIENCE AND TECHNOLOGY Meas.Sci.Technol. 14 (2003) 1487–1492 PII: S0957-0233(03)57428-8 Direct radiocarbon dating of prehistoric cave paintings by accelerator mass spectrometry Hel´ ene` Valladas Laboratoire des Sciences du Climat et de l’Environnement, Unitemix´ te CEA-CNRS, Batimentˆ 12, Avenue de la Terrasse, 91198 Gif-sur-Yvette Cedex, France Received 13 December 2002, accepted for publication 26 February 2003 Published 29 July 2003 Online at stacks.iop.org/MST/14/1487 Abstract Advances in radiocarbon dating by accelerator mass spectrometry now make it possible to date prehistoric cave paintings by sampling the pigment itself instead of relying on dates derived from miscellaneous prehistoric remains recovered in the vicinity of the paintings. Presented below are some radiocarbon dates obtained at the ‘Laboratoire des Sciences du Climat et de l’Environnement’ for charcoal used in the execution of prehistoric paintings decorating two French caves: Cosquer and Chauvet. The presentation of the dateswill be preceded by a short discussion of the experimental procedure used in our laboratory (pigment sampling, chemical treatment, etc). The ages obtained so far have shown that the art of cave painting appeared early in the Upper Palaeolithic period, much earlier than previously believed. The high artistic quality of the earliest paintings underlines the importance of absolute chronology in any attempt to study the evolution of prehistoric art. Keywords: AMS carbon-14 dating, prehistoric cave paintings, charcoal, Upper Palaeolithic, Cosquer cave, Chauvet cave 1. Introduction time of execution of the painting. Did the artists use freshly Until quite recently cave paintings were dated according to made charcoal, leftover material from prior cave occupation stylistic criteria loosely associated with dates obtained for (Bednarik 1994) or a mixture of charcoals of several origins? archaeological remains found in the vicinity of decorated The possibility that fossil charcoal could have been used surfaces. About two decades ago radiocarbon dating was cannot be excluded either (Bednarik 1994). To compound revolutionized when accelerator mass spectrometric (AMS) the problems there is also the possibility that some paintings techniques allowed for the dating of organic samples weighing were retouched by a later generation of artists. Some of as little as 1 mg. Paintings done in charcoal could now be these questions can be answered by examiningthenature sampled without visibly damagingthe paintings. In addition and composition of the pigment under a scanning electron to wood charcoal, which has received the most attention (Rowe microscope, others require meticulous in situ examination of 2001, Valladas et al 1992, Igler et al 1994), beeswax (Nelson thepigment layer with a good magnifying glass. et al 1995) and plant residues (Watchman and Cole 1993, The sampling, the first step of the dating process, is done Hedges et al 1998) used in the paintings have also been dated. after preliminary analysis has revealed that the black pigment Below we present theapproach used at the Laboratoire des contains charcoal. In some instances the wood could be Sciences du Climat et de l’Environnement (LSCE) to date identified as belonging to the species Pinus. Palaeolithic charcoal drawings and paintings and discuss the To protect the visual integrity of the drawings, pigment results obtained in two French caves. is scraped from rock cracks or from the thickest layers. If the charcoal is well preserved and thick enough, it is best 2. Problems peculiar to the dating of prehistoric to collect the sample from a limited area of a figure. When pigments possible, two or more samples from different portions of a The first problem, to which there is no simple scientific answer, painting should be taken in order to get several dates and check has to do with the question of the age of the charcoal at the the age spread. Otherwise, if the pigment layer is too thin and 0957-0233/03/091487+06$30.00 © 2003 IOP Publishing Ltd Printed in the UK 1487 HValladas SAMPLE PREPARATION The great majority of contaminants introduce carbon younger than the pigment charcoal and if not eliminated by a proper Acid (HCl, 0.5M) treatment will produce a date more recent than the true one. High-purity H2O 3. Sample treatment Deposition on pre-cleaned quartz filter The sample pre-processing used to date the Palaeolithic Basictreatment charcoal drawings and paintings has been described in recent Na4P2O7 ,NH3 (aq), NaOH publications (Valladas et al 1999, 2001a). The treatment of charcoal varies in intensity according to the sample size. It involves asuccession of ‘acid–base–acid’ treatments which Charcoal Humic fraction Acid (HCl, 1M) Precipitation and first dissolve the carbonates that may have come from the H2O collection on a limestone wall or ground water, then humic acids arising from quartz filter the transformation of organic matter, and bacteria or other living microorganisms. A schematic representation of the Drying Drying treatment steps is shown in figure 1. The residue from the initial acid bath is retained on a Heating, 1hr at 300 - 320°CHeating, 1hr at 280°C in a stream of oxygen in a stream of oxygen pre-cleaned quartz-frit filter and subjected to the subsequent basic treatment. This treatment, gentle at first, is increased in intensity according to the fragility of the sample. One begins with a dilute solution of sodium pyrophosphate whose concentration is increased progressively. Aqueous ammonia Sample transferred to a combustion tube containing of gradually increased concentration is used next, followed CuO and Ag wire and sealed under vacuum by sodium hydroxide treatment in cases of alkali-resistant pigments. As a rule, the treatment stops when the filtrate Oxidation at 850°Cfor 7 hours becomes highly coloured. The coloration suggests that not only have the outer grain layers been stripped, but that a good Purification and determination of CO2 pressure fraction of the original charcoal has passed into solution. If the Catalytic reduction to graphite treatment is not interrupted in time, no charcoal might be left for dating. The remaining charcoal grains are washed again Compression to a pellet used as target with aqueous HCl. After the chemical treatment, the purified charcoal or humic acids collected on another quartz filter are AMSmeasurement heated in a stream of oxygen for about an hour between 280 and 320 ◦Ctoremove some additional organic contaminants. Figure 1. Adiagram illustrating the experimental procedure. Whatever remains is oxidized to carbon dioxide, then reduced to graphite and compressed into pellets for the has to be scraped from several points, sometimes far apart, one accelerator (Arnold et al 1987). The purification process gets an average date. The collected samples, usually weighing eliminates more than 90% of the original mass leaving us with from 10 to 100 mg, often contain calcite grains or clay from pellets usually containing from 0.5 to 1 mg of carbon (tables 1 the rock face, in addition to wood charcoal. To-date, calcium and 2, column 3). oxalate, which can be an important contaminant (Watchman 1990, Russ et al 1996, Hedges et al 1998) of outdoor parietal This procedure has been tested on a piece of charcoal art in semi-arid regions (particularly in the vicinity of cacti, from an Upper Palaeolithic layer (Solutrean). The piece was lichens, for example), has not been detected in paintings inside broken into several subsamples, of which some were subjected West European caves. to very strong chemical treatment, others treated in the same Amajor problem, inherent in all methods of radiocarbon wayasthe pigment samples and still others subjected to dating, is the possible presence of extraneous carbon (Hedges chemical but not thermal treatment. We found that a strong et al 1989). Exposure of a paintings renders a cave painting’s chemical treatment did not give significantly different results pigment particularly vulnerable to contamination. The degree from the weaker treatment usually reserved for the paintings, of contamination depends on when and how the caves were and that the thermal treatment did eliminate some additional discovered. For obvious reasons, caves sealed until recently contamination by more recent carbon, since the samples thus and not open to the public should give the most reliable dates. treated gave slightly older ages. The results also confirmed the In caves frequently visited in the past the most common good reproducibility of our protocol (Valladas et al 2001a). organic contaminants come from contact with visitors’ hands, The extent of contamination by modern carbon during cloth fibres, acetylene lamp soot, etc. Moreover, all sample preparation was determined by subjecting several cavesharbour a variety of microorganisms whose growth is charcoals over 100 000 years old (‘blank’ sample without 14C) stimulated by emanations from the human body (Laiz et al to the same treatment as our pigment samples. This yielded 1999). One must also consider contamination by carbonic, background contamination that was used to make a suitable humic or fulvic acids transported by underground waters. correction to the calculated pigment ages. 1488 Direct radiocarbon dating of prehistoric cave paintings by accelerator mass spectrometry Table 1. Radiocarbon dates for prehistoric paintings at the Cosquer cave. Humic acid dates are written in italics. For pictures of the dated paintings see Clottes and Courtin (1994). Ly
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