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Known as lead white, lead carbonates were used as white pigment or cosmetics from the 4th century BC to the 20th century AD. Lead white was produced by the corrosion of metallic lead by vinegar and horse manure up to the 19th c. In order to document the incorporation of carbon in the corrosion mechanism, lead carbonates were produced in the laboratory under monitored experimental conditions using materials with different isotope signatures in 14C and 13C. Six experimental setups were defined combining vinegar, acetic acid, horse manure and fossil CO2 gas. The corrosion products were characterized by X-ray diffraction. 14C content and δ13C values of the initial reactants and the final products were measured by accelerator and isotopic ratio mass spectrometry (AMS and IRSM). The reaction between lead and vinegar or acetic acid resulted in lead acetates with a carbon isotopic signature close to that of the corrosive reagent. In the presence of CO2, the carbonatation reaction occurred and the cerussite produced had a predominant 14C signature of the carbon dioxide source. These experiments demonstrate that the CO2 produced by horse manure fermentation is incorporated into the corrosion products, allowing the absolute dating of lead white by the radiocarbon method.
Spermaceti is a waxy substance found in the head cavities of sperm whales (Physeter macrocephalus and P. catodon). This substance had a variety of commercial applications from the end of the 18th to the beginning of the 20th century, such as candles, soap, cosmetics and other compounds. Spermaceti was also occasionally used as wax for modeling sculptures. In order to date such artworks the marine reservoir effect (MRE) has to be considered. The chemical library of the Muséum national d’Histoire naturelle (Paris, France) contains samples of spermaceti studied by the French chemist M. E. Chevreul (1786–1889) at the beginning of the 19th century. Eight samples of substances preserved in their original containers were 14C dated. According to the whaling practices and the publications of Chevreul, we estimated that the spermaceti samples came from whales caught between 1805 and 1815. AMS 14C dating results are from 550 to 1180 ± 30 BP, R values between 393 and 1023 (± 34) 14C yr and ΔR between –168 and 504 (± 60) 14C yr. The values presented here are the first ever obtained for spermaceti. However, being based on museum specimens, further measurements on crude material would be necessary to refine these results.
The direct dating of rock paintings is not always possible due to the lack of organic carbon compounds in pigments, or because sampling from a heritage site is often restricted. To overcome these limitations, dating laboratories have to develop new approaches. In this study, we consider sampling calcium oxalate crusts covering the painted artworks as a way to indirectly date the rock art. This stratigraphic approach includes isolating and extracting pure oxalate from the crusts. The approach was tested on natural bulk accretions collected in the open-air sites of Erongo Mountains in Namibia. The accretions were separated into two phases (pure oxalate and the remaining residues) with a special pretreatment. This process removes carbonates through acidification (HCl 6N) and dissolves the oxalate into the supernatant, leaving the minerals and windblown organic compounds in the residue. The efficiency of the separation was checked on the two phases by FTIR analyses and by 14C dating and showed that pure oxalate powders were indeed obtained. AMS radiocarbon results of various accretions on the same art panels provided ages from modern periods to 2410 ± 35 BP. From these first results, more targeted sampling campaigns can be considered to provide a terminus ante quem for the rock art.
Quality control procedures have been developed at the Laboratoire de Mesure du Carbone 14 (LMC14) national laboratory throughout the years of operation. Routine procedures are applied to sample preparation depending on their composition and their size. The tuning of the ARTEMIS AMS facility, hosted by the LMC14 laboratory, uses an accurate procedure. A batch of unknown samples is measured with accompanying samples (primary and secondary standards and blanks), which give a powerful set of data to control the quality of each measurement. A homemade database has been created to store the sample information and study the evolution of the accompanying samples. The LMC14 laboratory participated in the Sixth International Radiocarbon Intercomparison, SIRI. The results are presented here, with statistical tests to assess the quality of the preparations and measurements done at the LMC14 national laboratory. To obtain a reliable radiocarbon (14C) age by AMS, 1 mg of sample is required in routine analysis. Recently, the LMC14 developed a new procedure dedicated to microsamples, allowing the size of samples to be reduced and contributing to opening 14C dating to materials that were previously unreachable. This new procedure has been successfully tested on valuable Cultural Heritage samples: lead white mural paintings.
The modern antiquities market uses radiocarbon (14C) dating to screen for forged objects. Although this fact shows the potential and power of the method, the circumstances where it is applied can be questionable and call for our attention. Here we present an outline of a call to radiocarbon laboratories for due diligence and best practice approaches to the analysis of antique objects requested by non-research clients.
Lead carbonates were used as cosmetic and pigment since Antiquity. The pigment, known as lead white, was generally composed of cerussite and hydrocerussite. Unlike most ancient pigments, lead white was obtained by a synthetic route involving metallic lead, vinegar and organic matter. Fermentation of organic matter produces heat and CO2 emission, leading to the formation of carbonates. As lead white is formed by trapping CO2, radiocarbon (14C) dating can thus be considered. We have developed a protocol to prepare lead white. We selected modern pigments for the experiment implementation and ancient cosmetic and paintings for dating. After characterization of the samples by XRD, thermal decomposition of cerussite at various temperatures was explored in order to select the appropriate conditions for painting samples. CO2 extraction yield, SEM and XPS were used to characterize the process. Thermal decomposition at 400°C was successfully applied to mixtures of lead white with other paint components (oil as binder, calcite as filler/extender) and to historical samples. We obtained radiocarbon measurements in agreement with the expected dates, demonstrating that thermal decomposition at 400°C is efficient for a selective decomposition of lead white and that paintings can be directly 14C-dated by dating lead white pigment.
JANNUS (Joint Accelerators for Nanosciences and Nuclear Simulation), the unique triple beam facility in Europe, offers the possibility to produce three ion beams simultaneously for nuclear recoil damage and implantation of a large array of ions for well-controlled modeling-oriented experiments. The first triple beam irradiation was performed in March 2010. Along with irradiation developments, continuous efforts have been made to implement ex situ and in situ characterization tools. In this study, we set out the present status of the JANNUS facility of the Saclay site. We focus on the instrumentation used for conducting multi-ion beam irradiations and implantations as well as for characterizing bombarded samples. On-line control of irradiation parameters, in situ modification monitoring using Raman spectroscopy or ion beam induced luminescence, and ex situ characterization by ion beam surface analysis [Rutherford backscattering spectrometry (RBS), nuclear reaction analysis (NRA), and elastic recoil detection analysis (ERDA)] of implanted samples are detailed. Some examples of single, dual, and triple beam irradiation configurations are presented. Access to the facility is provided by the French network EMIR for national and international users (http://emir.in2p3.fr/).
Direct dating of prehistoric paintings is playing a major role in Paleolithic art studies. Very few figures can be directly dated since the necessary condition is that they contain organic carbon-based material. Thus, it is very important to check the presence of organic carbon-based material in situ before sampling in order to protect the visual integrity of the paintings or drawings. We have tested and compared 3 different portable analytical systems that can be used in cave environments for detecting carbon in prehistoric paintings: (1) a very compact X-ray fluorescence (XRF) system in Villars Cave (Dordogne, France); (2) a portable micro-Raman spectrometer in Rouffignac Cave (Dordogne, France); and (3) an infrared reflectography camera in both caves. These techniques have been chosen for their non-destructiveness: no sample has to be taken from the rock surface and no contact is made between the probes and the paintings or drawings. The analyses have shown that all the animal figures have been drawn with manganese oxides and cannot be directly dated by radiocarbon. However, carbon has been detected in several spots such as black dots and lines and torch marks. 14C results were obtained from 5 torch marks selected in Villars Cave, with ages between 17.1–18.0 ka cal BP. Three methods were used to identify carbon in black pigments or to confirm the presence of torch marks by carbon detection. Thanks to these new analytical developments, it will be now possible to select more accurately the samples to be taken for 14C dating prehistoric paintings and drawings.
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