ESR/U-series dating of Eemian human occupations of Northern France

Palaeolithic sites associated with the Eemian Interglacial (MIS 5e) are very rare in NW Europe, and especially in Northern France, where their preservation is restricted to very specific geological contexts, in association with carbonated tufa (Caours) or peat deposits (Waziers). In order to check the reliability of ESR/U-series method to date teeth recovered from archaeological levels in such specific geological environments, teeth were sampled on these two Middle Palaeolithic sites and systematic in situ dosimetry was performed using portable gamma spectrometer. The ESR/U-series ages obtained on the Caours site are very homogeneous allowing the calculation of a mean age equal to 125 ± 11 ka, in agreement with the geological age, mammal's association and other available geochronological data (U-series on tufa carbonate, TL on burnt flints, OSL on sediments), despite a relatively heterogeneous dosimetric environment (gamma dose rate ranging between ca 200–450 μGy/a). At Waziers, reducing (water logging) environment linked to the peat leads to very specific U-series data of the analysed teeth (U content lower than 0.1 ppm in all the dental tissues, evidence of leaching in some tissues), but the mean ESR/U-series age, 129 ± 4 ka, is also in agreement with the available geological and palaeoenvironmental data indicating that the dated teeth were associated with Late Glacial deposits prior to the climatic interglacial optimum. These two case studies then confirm the reliability of ESR/U-series method to date with good reliability and accuracy the archaeological levels linked to such relatively short climatic events (ca 10 ka).     

The chronology of the late Lower Paleolithic in the Levant based on U–Th ages of speleothems from Qesem Cave,Israel

We present here the results of a U–Th dating project at Qesem Cave, a Middle Pleistocene, late Lower Paleolithic site in Israel. It provides 54 new MC-ICP-MS U–Th ages for speleothems from the cave. The results indicate that human occupation started sometime between ～420 and 320 ka and ended between 220 and 194 ka. A survey of dates from culturally similar sites in the Levant indicates that the general range of ca. 400–ca. 200 ka is an appropriate estimate for the life span of the Acheulo-Yabrudian Cultural Complex (AYCC).     

Applying a Bayesian approach for refining the chronostratigraphy of the Yumidong site in the Three Gorges region,central China

Yumidong (Corn Cave) is a newly discovered Paleolithic site in the Three Gorges region of central China. Numerous Paleolithic artifacts have been excavated from the sedimentary deposits of the cave in association with faunal remains attributed to the Middle-Late Pleistocene Ailuropoda-Stegodon fauna of southern China. To establish the chronology of the sedimentary sequence (>5 m thick), ¹⁴C dating was applied to bone and charcoal samples (n = 6); the U-series method was used to date in situ precipitated speleothems (n = 12), transported speleothem samples (n = 6) and 18 subsamples of a fossil tooth; and the coupled ESR/U-series method was used to date fossil teeth (n = 6). The derived dates were combined using a hierarchical Bayesian approach to generate a unified chronostratigraphy for the Yumidong sequence. In our Bayesian analyses, the ¹⁴C and coupled ESR/U-series dates were considered to provide direct age estimates for the target layers, while the U-series dates of the in situ precipitated speleothems and fossil tooth were used as minimum age constraints and those of the transported speleothem fragments as maximum age constraints. The Bayesian analyses provided robust time intervals for the archeological layers: L2-Upper (14–23 ka), L2-Lower (27–63 ka), L3 (106–171 ka), L4 (140–192 ka), L10 (157–229 ka), L11 (181–256 ka), and L12 (214–274 ka) with a probability of 95%, allowing the establishment of a ∼300 ka long geological and archeological history for the Yumidong site and placing it as a reference site for Paleolithic cultural evolution in the Three Gorges region from the late Middle Pleistocene to Late Pleistocene.     

ESR dating in Song Terus cave (East Java, Indonesia)

Electron spin resonance (ESR) dating on teeth has been used to determine the antiquity of the human presence in the area of Gunung Sewu (East Java, Indonesia). The Song Terus cave is one of the archaeological sites located in this area, which has yielded an important collection of fossil bones and prehistoric lithic industry. ESR dating shows that this cave belongs to a karstic system which has been in place since Middle Pleistocene. The results of coupled ESR/Uranium-series dating indicates closed system for uranium in tooth tissues yielding ages of between 216 and 392 ka for the oldest archaeological levels, confirming the possibility of finding Middle Pleistocene human occupations in such karstic sites in Java.     

Dating results on sedimentary quartz,bones and teeth from the Middle Pleistocene archaeological site of Coudoulous I (Lot,SW France): A comparative study between TT-OSL and ESR/U-series methods

This study presents palaeodosimetric results from the Middle Pleistocene archaeological site of Coudoulous I (Lot, SW France). Nine sedimentary quartz samples (41–60 μm) have been analyzed using a multiple aliquot protocol based on the measurement of the TT-OSL signal. In addition, 7 teeth and 7 bones have been dated by combining the ESR method with U-series analyses. Both methods gave consistent age results allowing correlation of the Early Middle Paleolithic Human occupation of the site to MIS 6 and part of the Lower Paleolithic tools to MIS 7. Beyond the establishment of a radiometric chronology for the Coudoulous I sequence, this study focuses on the information extracted from the intercomparison of the methods. Our data suggest that 1) the TT-OSL signal is stable over at least the last 230 ka (considering the age range of the studied samples), 2) there are not significant problems of incomplete bleaching leading support to the applicability of the TT-OSL technique for sedimentary deposits associated with karstic contexts. This approach highlights the interest of combining luminescence and ESR/U-series methods to discuss the reliability of the dating results.     

ESR/U-series dating of faunal remains from the paleoanthropological site of Biache-Saint-Vaast (Pas-de-Calais,France)

Discovered accidently during factory building construction works, the Middle Palaeolithic site of Biache-Saint-Vaast (Pas-de-Calais, France) was excavated from 1976 to 1982 by a team of Lille University directed by Alain Tuffreau. An abundant archaeological and paleontological material, including two human skulls, was there recovered from fossil alluvial deposits of the Scarpe River. In order to determine the ages of these remains, the ESR/U-series method was applied on bone and teeth. As the U-series data obtained of the main part of the analyzed tissues do not allow the use of the classical US-ESR model, the recently proposed AU-ESR model, taking into account if necessary U-leaching from some of the tissues, was used to calculate combined ESR/U-series ages for these samples. The obtained ages suggest a MIS7 attribution to the faunal remains and permit an age of ca 240 ka to be assigned for the human remains and associated archaeological material, in accordance with the stratigraphic data and the large mammal associations.     

New ESR and U-series dating at Caune de l'Arago,France: A key-site for European Middle Pleistocene

The Caune de l'Arago, located at Tautavel in the southern part of France, is one of the best documented Middle Pleistocene sites allowing a good understanding of human evolution in Europe. Since its discovery in 1829, the cave yielded more than 140 human remains associated with abundant lithic industries and thousands of faunal remains in a 10 m thick stratigraphical sequence divided in three complexes (Lumley et al., 2014). The Lower stratigraphic complex is only known from cores while the Middle and Upper ones can be divided into about 17 main archaeological levels indexed from the bottom to the top: from level Q to level A. Since 1981, a number of dates were done using practically all the methods available for dating Quaternary period up to 700 ka. U-series dates performed on the upper stalagmitic floor yielded a minimum age of 400 ka for human remains found in the underneath level G (Falguères et al., 2004). This age range confirmed the direct non-destructive gamma-ray age published more than 30 years before (Yokoyama and Nguyen, 1981). Recently, a methodological work was published on herbivorous teeth coming from different parts of the G level highlighting the difficulties to get reliable radiometric dates on a level so rich in bones and partly weathered by guano deposits or issues associated with carbonate accumulation (Han et al., 2010).This study presents new ESR/U-Series dates obtained on herbivorous teeth coming from the lowest excavated layers (Q–P levels) which yield an age range for the entire thick archaeological infilling. The new results suggest that the sedimentological levels containing lithic and faunal artefacts began to be deposited at 550 ka in the P–Q levels and a younger age of 350–400 ka for the F level. The P–Q levels which have yielded bifaces are one of the oldest evidence of the Acheulian culture in the southern part of Western Europe while the dates obtained on G level suggest a contemporaneity with la Sima de los Huesos and TD10 Dolina level at Atapuerca.     

40Ar/39Ar and ESR/U-series dates for Guado San Nicola,Middle Pleistocene key site at the Lower/Middle Palaeolithic transition in Italy

The Middle Pleistocene archaeological site of Guado San Nicola was discovered in 2005 in a fossil fluvial terrace of the Volturno River, close to the village of Monteroduni, Molise, Italy. Palaeontological remains and lithic artefacts, including both handaxes and Levallois, discoid and opportunistic debitage, were recovered in fluvial and slope sediments rich in volcanoclastic materials. This site includes four distinct human occupation levels. In two of them both “shaping-façonnage” and “knapping-débitage” technologies are highlighted, placing this site at the Lower/Middle Palaeolithic transition.In the present study, geochronological analyses by ⁴⁰Ar/³⁹Ar on single-crystal and ESR/U-series on teeth were performed to precise the chronological framework of the occupations. The ⁴⁰Ar/³⁹Ar data obtained securely bracket the human occupation levels at the transition between the interglacial and glacial marine isotopic stages MIS 11 (i.e. 400 ± 9 ka) and MIS 10 (i.e. 345 ± 9ka). The weighted mean age obtained from ESR/U-series dating of six teeth (i.e. 364 ± 36 ka) is in very good agreement with the ⁴⁰Ar/³⁹Ar results. The radio-isotopic constraints we presented place the Guado San Nicola site as one of the earliest testimonies of Levallois debitage in Western Europe and confirm the potential and accuracy of paleo-dosimetric methods to date Middle Pleistocene sites.     

Extended-range luminescence chronologies for the Middle Pleistocene units at the Sima del Elefante archaeological site (Sierra de Atapuerca,Burgos, Spain)

The Sima del Elefante site is located within the Sierra de Atapuerca karst system (Burgos, northern Spain), and forms part of a series of important Early, Middle and Late Pleistocene archaeological complexes that have been dated previously with luminescence techniques (Gran Dolina, Galería Complex, Sima de los Huesos, Galería de las Estatuas). This study focuses on the upper Middle Pleistocene units (TE18 and TE19) at Sima del Elefante, which contain Acheulean and transitional lithic assemblages (Mode 2/3), as well as large and small mammal fossils. Importantly, these uppermost units are associated with a sediment plug located in the cave's interior at Galería Baja, which marks the closure of a significant palaeoentrance to the Atapuerca karst system. Establishing the accumulation history of these related deposits is important for understanding both Lower Palaeolithic technological dynamics via comparisons with similar levels at other Atapuerca sites (i.e., Gran Dolina and Galería Complex), as well as past human occupation patterns and carnivore use of (and accessibility to) the caves. We present single-grain TT-OSL and multi-grain pIR-IR chronologies for the Sima del Elefante upper sequence and the Galería Baja sediment cone, as well as U-series dating results for a stalagmitic crust capping the combined clastic infill sequence. The paired luminescence ages for the upper occupation levels are in agreement with each other and reveal that the host deposits accumulated 576–481 ka for the TE18 stratified scree layers, 266–237 ka for TE19 and 206–250 ka for the Galería Baja upper cone section (weighted mean 2σ age ranges). A concordant U-series age of 202 ± 65 ka is obtained for the overlying stalagmitic crust at Galería Baja. The Sima del Elefante ages are consistent with those previously obtained using U-series and biochronology, confirming that there is an erosional unconformity and complex carbonate deposition phase associated with the upper layers of unit TE18 and that the original cave entrance likely closed by ∼200 ka. Chronological correlation with other Atapuerca sites reveals potential equivalence between TE18 and unit TD8 (at Gran Dolina), and between TE19 and units GIIb–GIIIb (at Galería Complex) and, possibly, TD10.1 and TD10.2 (at Gran Dolina), though more refined dating is required to confirm the latter.     

Coupled ESR and U-series dating of early Pleistocene Gigantopithecus faunas at Mohui and Sanhe Caves,Guangxi, southern China

Several caves of the Guangxi Zhuang Autonomous Region, southern China, have delivered Gigantopithecus blacki remains, an extinct Pleistocene giant ape, in association with abundant mammalian faunas. To determine their geological ages, fossil teeth from Mohui and Sanhe Caves were dated using the coupled ESR/U-series method. The teeth from Mohui Cave gave age estimates of 1.69 ± 0.22 Ma and 1.29 ± 0.11 Ma. The Sanhe Cave samples had age estimates ranging from 910 ± 200 ka to 600 ± 150 ka with error weighted mean ages of 890 ± 130 ka and 720 ± 90 ka for the layers 5 and 4, respectively. Our results and previous paleomagnestism data place the Gigantopithecus fauna at Mohui Cave between Olduvai and Jaramillo subchrons and suggest that it was coeval with Chuifeng, Longgupo and Liucheng assemblages. The Sanhe fauna is younger, of late early Pleistocene age, and can be dated to the period between Jaramillo subchron and B/M boundary.     

Radiometric dates for the Middle Palaeolithic sequence of Payre (Ardèche, France)

The archaeological site of Payre (France) yielded Middle Palaeolithic layers with Neanderthal remains, which are partly bracketed by two stalagmitic flowstones. To obtain a precise chronological framework for the human occupation and the faunal remains of this site, several dating methods were used: uranium-series (U-series by alpha spectrometry and TIMS) and electron spin resonance (ESR) on stalagmitic flowstones, combined ESR/U-series on teeth and bones, and thermoluminescence (TL) on burnt flints. Most of the ages obtained for levels H to C range from 300 to 140 ka. The age-spread obtained for the anthropic (burnt flints) and faunal remains (bones and teeth) suggests that the dated levels represent several human occupation periods, near the transition from MIS8 to MIS7 (levels G–F) and from MIS6 to MIS5 (levels D–E).     

Radiometric dating of Meipu hominin site in China by coupled ESR/U-series and cosmogenic 26Al/10Be burial dating methods

The Three Gorges and Western Hubei area in the geographic central part of China was a potential migration corridor for early hominin and mammals linking South and North China during the Pleistocene period. Some key early hominin sites are known in this region where limestone cave and fissure sites are numerous but difficult to date as beyond the dating range of OSL and mass spectrometry U-series method. Here, we report radiometric dating study for such a hominin site, Meipu (Hubei Province), by coupled ESR and U-series dating of nine fossil teeth and cosmogenic ²⁶Al/¹⁰Be burial dating of one quartz sediment. The burial age calculated by simple burial model (573 ± 266 ka) gives a minimum age constraint of the sediment. The fossil dating provided two main age groups at 541 ± 48 ka and 849 ± 39 ka, the older age group is in agreement with the U-series age (>630 ka) of the flowstone overlying the fossil layer and the paleomagnetic data which placed the Brunhes-Matuyama boundary in the fossil layer. The reason of this age difference is probably caused by the U-content discrepancy in the enamel of the dated fossil samples. This study exhibits the limitation of ESR/U-series fossil dating and the importance of using multiple dating approach when it is possible in order to identify the problematic ages.     

ESR/U-series dating of teeth recovered from well-stratigraphically age-controlled sequences from Northern France

During the last two decades, extensive road-construction works in Northern France have allowed the discovery of numerous Middle Palaeolithic sites. Geological and multidisciplinary studies performed on these localities allowed the establishment of a precise chronostratigraphical and biostratigraphical framework of regional significance, which could be correlated to the global marine palaeoclimatic scale. Each human occupation layer has been linked to this regional framework, thus providing a stratigraphical age-control for the Middle Palaeolithic human settlements of this area.At the same time, a program of geochronological studies was developed using TL, OSL, U-series, ESR and, as often as possible, ESR/U-series methods. Hence, bones and teeth recovered from archaeological sites of Savy, Ault, Caours, Gentelles and La Celle-sur-Seine, were analyzed and the results compared to the chronostratigraphical ages. The age results are generally in good agreement with the geological data while bones and dental tissues display in some cases U-series ages higher that the EU-ESR ones, suggesting U-loss phenomena.     

ESR chronology of the Somme River Terrace system and first human settlements in Northern France

The Somme Valley, Northern France, is famous for its archaeological sequence, where numerous rich Palaeolithic sites, such as Saint-Acheul, the type site of the Acheulian, have been discovered. The archaeological levels are often directly associated with fossil alluvial sediments of the River Somme or with slope deposits, including loess and palaeosols. In the middle reaches of the valley, near Amiens, the system of fossil-stepped fluvial terraces is particularly well developed and preserved, and occurs on 10 alluvial formations. These terraces, from +5 to +55 m above the present-day valley bedrock, allow the study of the environmental changes and the human settlement of this area through the Pleistocene.

Since 1988, ESR dating was systematically applied on bleached quartz extracted from the fossil fluvial deposits, in order to better describe the geological evolution of the stepped system. More recently, U-series/ESR dating has also been performed on teeth collected from the different terrace deposits. Here we present a synthetic review of the main ESR results, and propose an ESR chronology for the geological evolution of the Somme fluvial system and for the Middle Pleistocene human settlement of northern France.     

Optical dating of flowstone and silty carbonate-rich sediments from Panxian Dadong Cave,Guizhou, southwestern China

Panxian Dadong Cave located in the western Guizhou is a very important Paleolithic site in China. At this site bone and stone artifacts, human teeth and mammalian fossils (known as Ailuropoda-Stegodon fauna) were found, and the site was previously dated to 120–300 ka using ESR/uranium-series methods. In this study, we successfully extracted fine quartz grains from flowstone and silty carbonate-rich sediments in the excavated area. The quartz extracts displayed excellent luminescence properties, and satisfied the SAR (single-aliquot regenerative dose method) acceptance criteria. The sensitivity-corrected OSL signals are not saturated at a dose up to about 1400 Gy. The cultural unit was OSL dated to 190–300 ka, corresponding to MISs 7–8. The flowstone deposits overlying the cultural unit were determined to be 13–190 ka and the silty carbonate-rich sediments underlying the cultural unit to be 300–360 ka. The optical ages are in general agreement with the coupled ESR/U-series and U-series ages.     

On the interest and the limits of using combined ESR/U-series model in the case of very late uranium uptake

Before ESR/U-series models were applied to ungulate teeth, it is generally assumed that calculated ages are close to the “real” ages when they range between the values obtained with the EU and LU models. When the samples show signs of uranium-leaching, a realistic mathematical modelling of the age is not possible. On the other hand, some samples have undergone a very late U-uptake “affecting” directly the U-series ages and rendering the calculated ages younger.

We present results obtained on two open-air sites, which show the limits of such combined models in the case of late uranium incorporation. For the Middle Pleistocene site of Isernia la Pineta (Italy), the ESR dates are expected to fall within the limits imposed by the Ar–Ar results. The other site, the Lower Palaeolithic deposits of Ambrona (Spain), yielded two sets of samples: some at the top of the sequence with uranium uptake ranging between EU and LU limits and thus giving a good idea of the “real” age of the site; others at the base displaying a very late U-uptake, which render an age determination difficult.     

High-precision U-series measurements of more than 500,000 year old fossil corals

Robust, independent age constraints on the absolute timing of climate events based on the U-series dating of fossil coral are sparse before the last glacial cycle. Using multiple-collector inductively coupled plasma mass spectrometry with multiple-Faraday protocols, we are able to date ～ 600 ka samples with an uncertainty of better than ± 15 ka (2σ), representing a three-fold improvement in precision compared with previous techniques. Using these methods, we report U-series measurements for a suite of > 500 thousand year old (ka) corals from Henderson Island, an emergent atoll in the south-central Pacific Ocean. The fossil corals show extraordinarily little diagenetic alteration for their age and the best-preserved sample yields a U-series age of 600 ± 15 ka (2σ), which overlaps with the timing of the warm Marine Isotope Stage (MIS) 15 interglacial. The open-system model of Villemant and Feuillet [Villemant B. and Feuillet N. (2003) Dating open systems by the ²³⁸U–²³⁴U–²³⁰Th method: application to Quaternary reef terraces. Earth and Planetary Science Letters 210(1–2), 105–118.] and the linear regression (or open-system isochron) is clearly limited for such old samples. However, the open-system model developed by Thompson et al. [Thompson W.G., Spiegelman M.W., Goldstein S.L., and Speed R.C. (2003) An open-system model for U-series age determinations of fossil corals. Earth and Planetary Science Letters 210(1–2), 365–381.] appears to reliably correct for open-system effects in roughly half of the corals, giving a MIS 15 origin for these. Thus the data provide evidence that the systematic addition of ²³⁰Th and ²³⁴U through α-recoil is a dominant open-system process occurring in the Henderson Island fossil reef system. Several coral samples yield significantly older Thompson et al. open-system ages between 650 and 750 ka. The uncertainty on these ages (typically ± 30 kyrs) is too great for precise assignment but most data overlap with the MIS 17 interglacial. The reliability of these ages is currently unclear. It is shown that separate aliquots of the same coral can yield different Thompson model ages. Therefore, there appear to be additional diagenetic mechanisms that create further anomalous excursions in the U-series systematics, limiting the reliability of the Thompson et al. open-system model.     

ESR/U-series chronology of the Neanderthal occupation layers at Galería de las Estatuas (Sierra de Atapuerca,Spain)

The Galería de las Estatuas is a Mousterian site located within the Cueva Mayor-Cueva del Silo karstic system at the Sierra de Atapuerca (Burgos, Spain). This site is characterised by an important Upper Pleistocene stratigraphic sequence in which a large number of lithic artefacts exhibiting clear Mousterian affinities and a rich assemblage of faunal remains have been found.Additionally, this site has yielded a foot phalanx of a clear Neanderthal affinities and its sediment has yielded Neanderthal mitochondrial and nuclear DNA.Two test pits, GE-I and GE-II, have been excavated since 2008 which have been divided in 5 and 2 lithostratigraphical units, respectively. A minimum age of 45 ka cal BP for this site was obtained by radiocarbon dating in GE-II. This chronology was refined using single-grain Optically Stimulated Luminescence (OSL: 80–112 ka in GE-I and 70–79 ka in GE-II) and single-grain thermally transferred OSL (TT-OSL). Although in all case TT-OSL ages were systematically older than their single-grain counterparts. The detrital sequence is sealed by a flowstone whose base is dated to 53.7 ± 3.5 ka cal BP using U-series dating.In order to better constrain the age of this site, nine herbivorous teeth were collected from the whole sedimentary sequence to be dated by the ESR/U-series dating method though only seven provided modelled ages. Six of them were collected from levels 2 to 5 of the GE-I test pit while the last tooth was taken from level 2 of the GE-II test pit. Our results, ranging between 80 and 110 ka, are in agreement with those obtained by single grain TT-OSL and suggest that the sedimentological levels containing Mousterian lithic artefacts and faunal and human remains began to be deposited during the second part of the MIS5. These results fill a temporal gap in the chronology of the Atapuerca sites for which no contemporary MIS5 date was obtained until recently.     

Investigating the effect of diagenesis on ESR dating of Middle Stone Age tooth samples from the open-air site of Lovedale,Free State,South Africa

Teeth are usually targeted for dating archaeological sites because they are less prone to dissolution, in comparison with bones. However, despite this apparent resistance, teeth do undergo diagenesis, which needs to be accounted for in order to obtain accurate ages. In particular, the uptake of trace elements such as uranium in dental tissues needs to be considered for dose rate determination when dated using electron spin resonance (ESR). Characterising the mineralogy and structural integrity of samples prior to dating may thus provide important information related to their state of preservation, especially in the case of teeth whose U content can significantly affect the dose rate.In this study, we dated five teeth of small-sized bovids using combined ESR/U-series dating. They were collected at the Middle Stone Age site of Lovedale, located in the central interior of South Africa. Micromorphology provided sedimentary context to the samples, which were recovered from a layer of gravel rich in faunal remains. Using cathodoluminescence, laser-induced fluorescence, Fourier transform infrared spectroscopy and Raman micro-spectroscopy we assessed the degree of preservation of the enamel. Results reveal that carbonate hydroxyapatite underwent post-depositional alteration, based on its molecular structure and elemental composition. Although the teeth all originate from the same layer and were sampled in the same 1-m square and at a similar elevation, U-content in the enamel differs highly from one tooth to the other, with values ranging from 1.7 to 29.6 ppm. These values are correlated with equivalent doses (D_e) from 228 to 923 Gy and are consistent with variations in crystallinity determined with vibrational spectroscopy. We also investigated the possible saturation of the ESR signal, by repeating measurements with microwave power values from 1 to 20 mW.Despite such diversity in U-content, the ages calculated assuming an early uptake of U all fall within the same range, from 63 ± 8 ka to 68 ± 15 ka and may only represent a minimum estimate.