The absolute dating of mortar by accelerator mass spectrometry (AMS) has been the subject of renewed interest for several years. International intercomparison campaigns, called MODIS (MOrtar Dating Intercomparison Study), have been carried out. The first MODIS-1 campaign highlighted limitations in mortar dating, due to the similarity between the primary material to be dated (binder) and the contaminant (exogenous CaCO3). Methods have since emerged to overcome this problem and the need for a good preliminary characterization has been proven. The Laboratoire de Mesure du Carbone 14 (LMC14) took part in the second intercomparison campaign, MODIS2, by applying thermal decomposition increments to distinguish the carbonated binder, the organic matter contaminants (late in formation pyrogenic carbonate, LDH) and limestone. The LMC14 results on MODIS2 are quite conclusive on “pure” re-carbonated lime mortar binders containing little contaminant geological limestone but show their weaknesses for mortars heavily contaminated in Dolomites, which are difficult to discern from the binder. Recommendations for users of radiocarbon (14C) dating on mortar-based materials are made in the conclusion.

In urban environments, diachronic evolution of water quality can be reconstructed using geochemical analysis of urban secondary carbonate deposits (USCDs), from urban underground structures, similar to speleothems from natural caves. The use of the radiocarbon bomb peak to build their precise chronology was recently tested in two Paris-area urban sites (France). In this study, new samples from contrasted environments in the Paris region were sampled in order to test the sites’ effects on the radiocarbon signal recorded: under wood, under a fountain, in underground aqueducts, in the south and north of Paris. We compared the post-bomb atmospheric radiocarbon record with the one measured at the top of USCDs, and estimated the dead carbon proportion (DCP), between 0 and 40%. USCDs fed by water with a rapid transfer through thin soil (Versailles fountain) had the lowest DCP (14C very close to atmospheric one). Highest DCP were found for USCD from deep underground quarry under urban wood, and intermediate ones for USCDs fed by the waters of perched aquifers. These data support the use of radiocarbon as chronometer for USCDs in contrasted urban contexts, and show that it can be used to determine carbon transport and sources, an important parameter for pollution reconstruction.

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.

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.

14C and U/Th methods were used to date three thin carbonate layers deposited on decorated walls of Nerja Cave (Malaga, southern Spain) in order to constrain the age of the parietal non-figurative marks situated under these carbonate layers. Modern formations were also dated to estimate the detritic contribution for the U/Th method and the dead carbon proportion for 14C dating. We sampled two locations with ocher painting marks. In one case (mark 1), the good agreement between the ages obtained by the two methods suggests that the sample was not subjected to post-deposition alteration and that the results are reliable. In the other case (mark 2), the age discrepancy between the two methods reached 30,000 yr, indicating that geochemical alteration had affected the sample and that one or both results were inaccurate. The ages for mark 1 indicate that this type of non-figurative representation is older than 25,000 cal BP and that it can be associated with the oldest attested Paleolithic occupation of Nerja Cave.

The nature and timing of environmental changes throughout the last glacial-interglacial transition in the South Caucasus, and more widely in eastern Europe, are still not fully understood. According to certain pollen records, forest expansion occurred in many areas several millennia after what is considered worldwide as the onset of the Holocene. The current problem we face is that the time lag in forest expansion varies from one sequence to another, sometimes with no delay at all. Moreover, the potential forcing/controlling factors behind this complex pattern, contrary to the almost synchronous global Holocene warming, are still a matter for debate. Accordingly, we revisit the issue of forest expansion through vegetation history obtained in the South Caucasus using a new pollen record, retrieved from the Nariani paleolake (South Georgia). These data attest to a steppic phase, initially dominated by Amaranthaceae-Chenopodiaceae (12,700–10,500 cal yr BP), then by Poaceae (10,500–9000 cal yr BP), culminating with a more forested phase (9000–5000 calyrBP). Although some palaeoclimatic regional reconstructions show a wet early Holocene, we interpret the delay in forest expansion recorded in Nariani (2500 years) as the result of reduced spring precipitation, which would have limited forest development at that time.