ABSTRACT The Laboratoire de Mesure du Carbone 14 (LMC14) has operated a radiocarbon dating laboratory for almost twenty years with ARTEMIS, the Accelerator Mass Spectrometer (AMS) based on a NEC 9SDH-2 Pelletron tandem accelerator. A first status report describing the chemical pretreatment methods was published in 2017 (Dumoulin et al. 2017). This article summarizes updates of the routine procedures and presents new protocols. The quality checks in place at the LMC14 and results obtained for the GIRI international inter-comparison are reported. New protocols developed by the laboratory over the last five years are described with the preparation of iron, lead white, cellulose, calcium oxalate, and mortar. This report also provides a summary of practical information for sample preparation and can help the laboratory users who provide samples and publish results to better understand all the work behind a 14 C dating.

ABSTRACT In 2001, five French public organizations (CNRS, CEA, IRD, IRSN, and the Ministère de la Culture) signed an agreement to purchase a new accelerator mass spectrometer to provide radiocarbon dating services at the national level. The Laboratoire de Mesure du Carbone 14 (LMC14) was set up in Saclay (France) around ARTEMIS, an AMS system based on a 3MV Pelletron from NEC and installed in early 2003. In 2015, the LMC14 joined the Laboratoire des Sciences du Climat et de l’Environnement, making it possible to develop research projects in addition to the service activity and since 2021, the LMC14 has been a member of the IAEA Collaborating Centre “Atoms for Heritage” at the Université Paris-Saclay. Since 2003, 70,000 samples have been measured. Two-thirds of the samples have been prepared on site and one-third in two associated laboratories in Paris and Lyon. Over the past years, the LMC14 has participated in several international inter-comparisons and has continuously improved its capabilities by developing new protocols for preparation and measurement. In this paper, the radiocarbon dating services of the last 20 years for research institutions, museums and environmental monitoring are reviewed and recent results from environmental and archaeological research programs are highlighted.

Two stalagmites from Nerja cave (Andalusia, Spain) were studied. The cave is well known because of its long human occupation from the Upper Palaeolithic to the Chalcolithic and its abundant parietal prehistoric Art. The aims of this study were twofold: i) to compare uranium/thorium (Th-230/U-234) and Carbon-14 (C-14) ages obtained all along the growth axis of the stalagmites in order to understand the consequences of diagenetic processes on the validity of radiometric ages; ii) as one of the stalagmites contains black layers, attributed to combustion soot, to establish when these intense hearths were used and by which culture. Th-230/U-234 and C-14 ages were coupled with mineralogical studies using FTIR (Fourier-transform infrared spectroscopy) and thin section observations. The first stalagmite (GN16-9b) displays Th-230/U-234 ages in stratigraphic order, and compatible with C-14 ages corrected for a few percent of dead carbon. Homogeneous composition of aragonitic crystals characterized by their needle-like texture is observed throughout this speleothem. For the second stalagmite (GN16-7), in contrast,Th- 230/U-234 ages display large significant inversions and discordant results on the upper part and at the base of the stalagmite, suggesting a possible open system behavior for this chronometer. Interestingly, 14C ages are in stratigraphic order all along the stalagmite and are compatible with Th-230/U-234 ages only in its central part. Mineralogical studies display evidence of aragonite to calcite transformation at the top and a complex mineralogical assemblage with interlayered silicates (possibly clays) and calcitic mineralogy for the base of GN16-7. In these parts, discordant Th-230/U-234 ages were measured. In the middle part of the stalagmite, however, where the fibrous aragonite is well preserved, the 14C and Th-230/U-234 ages agree. Our data suggest that in the case of aragonite to calcite transformation as shown here, Th-230/U-234 ages are biased, but C-14 ages seem to remain accurate, as already observed in aragonitic marine bio minerals. C-14 ages obtained are used for the chronology of the soot layer, determined here between 7900 and 5500 years Cal BP, coherent with previous analysis of charcoals in the same sector of the cave. This study highlights the importance of working with at least two chronometers when stratigraphic age verification is not possible, as is the case of some parietal CaCO3 thin layers used for rock art dating. Recent Th-230/U-234 ages published for carbonate deposits on Spanish parietal Art are discussed in light of this demonstration. (C) 2022 Elsevier Ltd. All rights reserved.

ABSTRACTEstuaries and deltas are crucial zones to better understand the interactions between continents and oceans, and to characterize the mineralization and burial of different sources of organic matter (OM) and their effect on the carbon cycle. In the present study, we focus on the continental shelf of the northwest Mediterranean Sea near the Rhône river delta. Sediment cores were collected and pore waters were sampled at different depths at one station (Station E) located on this shelf. For each layer, measurements of dissolved inorganic carbon concentration (DIC) and its isotopic composition (δ13C and Δ14C) were conducted and a mixing model was applied to target the original signature of the mineralized OM. The calculated δ13C signature of the mineralized organic matter is in accordance with previous results with a δ13COM of marine origin that is not significantly impacted by the terrestrial particulate inputs from the river. The evolution with depth of Δ14C shows two different trends indicating two different Δ14C signatures for the mineralised OM. In the first 15 cm, the mineralized OM is modern with a Δ14COM = 100 ± 17‰ and corresponds to the OM produced during the nuclear period of the last 50 years. Deeper in the sediment, the result is very different with a depleted value Δ14COM = –172 ± 60‰ which corresponds to the pre-nuclear period. In these two cases, the marine substrate was under the influence of the local marine reservoir effect with more extreme Δ14C results. These differences can be largely explained by the influence of the river plume on the local marine DIC during these two periods.

ABSTRACT Very little is known about the manufacturing and use of ancient Egyptian instruments, and their discovery is very rare. An extensive radiocarbon ( 14 C) dating program has been conducted on 25 ancient Egyptian musical instruments currently held at the Louvre Museum ( musée du Louvre ) and the Lyon Museum of Fine Arts ( musée des Beaux-Arts de Lyon ). This study includes cordophones (harps, lyres, lutes), membranophones (drums, tambourines), idiophones (clappers, crotales), as well as wind instruments (oboe) that have entered the museum collections during the 19th century or the first half of the 20th century; consequently, the original archaeological contexts of their discoveries are poorly understood. Approximately 50 14 C dates enable drawing a general overview of the instruments manufacturing. A wide variety of wood material has been identified, representing both indigenous species and imported species. Results indicate that the native flora of Egypt was exclusively used until the Third Intermediate Period when the first imports could be identified. 14 C results are not always consistent with relative dates previously thought, mainly based on stylistic criteria. They demonstrate these collections hold very well-preserved objects extending over 2500 years, from the Second Intermediate Period (ca. 1700 BCE) to the start of the Islamic Period (8th century CE). This project provides important results for the knowledge of ancient Egyptian musical instrument crafts.

ABSTRACTA better understanding of the dynamics of different particulate organic matter (OM) pools in the coastal carbon budget is a key issue for quantifying the role of the coastal ocean in the global carbon cycle. To elucidate the benthic component of this carbon cycle at the land-sea interface, we investigated the carbon isotope signatures (δ13C and ∆14C) in the sediment pore waters dissolved inorganic carbon (DIC) in addition to the sediment OM to constrain the origin of the OM mineralized in sediments. The study site is located at the outlet of the Rhône River (Mediterranean Sea), which was chosen because this river is one of the most nuclearized rivers in Europe and nuclear 14C can serve as a tracer to follow the fate of the OM discharged by the river to the coastal sea. The ∆14C results found in the pore waters DIC show a general offset between buried and mineralized OM following a preferential mineralization model of young and fresh particles. For example, we found that the sediment OM has values with a mean ∆14C=–33‰ at sampling stations near the river mouth whereas enriched ∆14C values around +523‰ and +667‰ respectively were found for the pore waters DIC. This indicates complete mineralization of a riverine fraction of OM enriched in 14C in the river conduit during in-stream photosynthesis. In shelf sediments, the ∆14C of pore waters DIC is slightly enriched (+57‰) with sediment OM reaching –570‰. A mixing model shows that particles mineralized near the river mouth are certainly of riverine phytoplanktonic origin whereas OM mineralized on the shelf is of marine origin. This work highlights the fact that pore waters provide additional information compared to sediments alone and it seems essential to work on both pools to study the carbon budget in river prodelta.

The hoard of Preuschdorf is a monetary deposit discovered in Alsace (France) in 2005. This find was composed of 7327 silver-copper coins. They seem to have been struck over more than one century, between the end of the 15th and the beginning of the 17th century. This hoard is an exceptional find composed of a large quantity of coins from various periods, areas and contexts. It is also remarkable by the presence of counterfeit coins.

AbstractThe main objective of this report is to present the dating process routinely applied to different types of samples at the Laboratoire de Mesure du Carbone 14 (LMC14). All the results and protocols refer to our procedures over the last 5 years. A description of the sorting and chemical pretreatments of the samples as well as the extraction and graphitization of CO2 are reported. Our last study concerning the degradation of the blank level according to the storage time of the targets between graphitization and accelerator mass spectrometry (AMS) measurement is also presented. This article also provides information on how to submit a valid laboratory sample. We give details relating to sampling procedures on site as well as contamination issues relative to the 14C dating methodology.

ABSTRACTIn this paper, first results comparing modified Longin and ninhydrin collagen extraction methodologies are presented. The goal of this study is to investigate the bones of several species with different ages, preservation conditions, and collagen contents to determine the most suitable preparation method. Different types of samples are used such as VIRI samples, previously dated bones, and background samples. Each bone has undergone elemental analysis, infrared analysis, and 14C measurement. The results are presented and the advantages and disadvantages of each preparation method are discussed. In general, results obtained by the two methods are in accordance with the consensus value for 2σ uncertainty. For VIRI I and a mammoth bone, the ninhydrin preparation gives, respectively, 8450±70 BP and 14,870±60 BP whereas the modified Longin process gives 8365±45 BP and 14,750±100 BP in agreement with the expected values. From the experimental point of view, the modified Longin process is easier to implement than the ninhydrin protocol. From this approach, we can conclude that the modified Longin process could be preferred in most cases and particularly when the amount of bone is small and the sample is not too contaminated.

The Artemis accelerator mass spectrometry (AMS) facility is dedicated to high-precision radiocarbon measurements. It routinely measures over 4500 samples a year for French laboratories. This paper is a status report, showing the measurements of standard, blank, and FIRI intercomparison samples. Since 2008, research and development programs have been established by the Artemis team. During the collaborations with other research laboratories, intercomparisons on archaeological samples were performed and are listed here to show the quality of the Artemis measurements. Three areas of specific research and development are investigated: technical development, beam optic simulations, and specific archaeological studies. The technical developments of the facility are based on the setup of a new bench for water sample preparation and routine microsample preparation and measurement. Beam optic simulations are carried out to control the quality of the measurement related to the tuning of the facility. International collaborations are always in progress. In 2012, the programs include improving the accuracy of reigns for the dynastic Egypt period and the 14 C dating of ancient iron.

The Artemis accelerator mass spectrometry (AMS) facility is dedicated to high-precision radiocarbon measurements. It routinely measures over 4500 samples a year for French laboratories. This paper is a status report, showing the measurements of standard, blank, and FIRI intercomparison samples. Since 2008, research and development programs have been established by the Artemis team. During the collaborations with other research laboratories, intercomparisons on archaeological samples were performed and are listed here to show the quality of the Artemis measurements. Three areas of specific research and development are investigated: technical development, beam optic simulations, and specific archaeological studies. The technical developments of the facility are based on the setup of a new bench for water sample preparation and routine microsample preparation and measurement. Beam optic simulations are carried out to control the quality of the measurement related to the tuning of the facility. International collaborations are always in progress. In 2012, the programs include improving the accuracy of reigns for the dynastic Egypt period and the 14C dating of ancient iron.

The Artemis accelerator mass spectrometry (AMS) facility, installed in 2003 in Saclay, France, is devoted to radiocarbon measurements. Samples are submitted by scientists in the fields of Quaternary geology, environmental sciences, and archaeology. The entire preparation process, originally optimized for samples with about 1 mg of carbon, has been tested in recent years for samples with a lower carbon content. In particular, we prepared and measured carbonate and organic background and reference samples ranging in mass from 0.01 to 1 mg C. These tests helped define our protocol's practical limits and determine necessary improvements. Furthermore, our experiments demonstrated that satisfactory graphitization yields (80% and higher) and low background values can be obtained with samples down to 0.2 mg of carbon. For handling smaller samples, we developed a specific process. We tested smaller reactors (5 mL in volume) and adapted the reduction parameters (H 2 pressure and temperature) accordingly. We also tested the effect of a chemical water trap on graphitization yields and 14 C results. This paper presents in detail the aforementioned developments and reports the 14 C results obtained for background and standard small samples prepared with the modified reactors.

We present here the new line installed at the LMC14 laboratory (Saclay, France) for dissolved inorganic carbon (DIC) extraction from marine and freshwater samples. The operating system and extraction process are described. The efficiency of the line design was checked, and the background (0.42 ± 0.11 pMC) and the reproducibility on artificial samples obtained by dissolution of IAEA-C1, IAEA-C2, and commercial bicarbonate in water were evaluated. An intercomparison with an independent lab (IDES) was also carried out on a natural sample. The line processes 3 samples a day under a helium flow and is able to run samples up to 40,000 ka.

The ARTEMIS facility in Saclay France measures, on average, 4500 samples a year for French organizations working in an array of fields, including environmental sciences, archeology and hydrology. In response to an increasing demand for the isolation of specific soil compounds and organic water fractions, we were motivated to evaluate our ability to reduce microgram samples using our standard graphitization lines and to measure the graphite thus obtained with our 3MV NEC Pelletron AMS. Our reduction facility consists of two fully automated graphitization lines. Each line has 12 reduction reactors with a reduction volume of 18ml for the first line and 12ml for the second. Under routine conditions, we determined that we could reduce the samples down to 10μg of carbon, even if the graphitization yield is consequently affected by the lower sample mass. Our results when testing different Fe/C ratios suggest that an amount of 1.5mg of Fe powder was ideal (instead of lower amounts of catalyst) to prevent the sample from deteriorating too quickly under the Cs+ beam, and to facilitate pressing procedures. Several sets of microsamples produced from HOxI standard, international references and backgrounds were measured. When measuring 14C-free wood charcoal and HOxI samples we determined that our modern and dead blanks, due to the various preparation steps, were of 1.1±0.8 and 0.2±0.1μg, respectively. The results presented here were obtained for IAEA-C1, 14C-free wood, IAEA-C6, IAEA-C2 and FIRI C.

The new facility Artemis was installed in 2003 in Saclay, France. This 3MV NEC Pelletron is dedicated to high-precision radiocarbon measurements for French 14C laboratories. We will present information on Artemis along with our sample preparation methods. Results from measurements on some intercalibration samples will be given along with the val- ues of measured blanks. Finally, we report on some problems we have encountered when measuring sputter cathodes with high CH- outputs.

The new facility Artemis was installed in 2003 in Saclay, France. This 3MV NEC Pelletron is dedicated to high-precision radiocarbon measurements for French 14C laboratories. We will present information on Artemis along with our sample preparation methods. Results from measurements on some intercalibration samples will be given along with the values of measured blanks. Finally, we report on some problems we have encountered when measuring sputter cathodes with high CH− outputs.