Luminescence and ESR dating of the sedimentary infill from the multi-level cave system of Alkerdi-Zelaieta (Navarre,N Spain)

The finding of Upper Paleolithic engravings in 2016 triggered a multidisciplinary investigation of the Alkerdi cave system (Urdazubi, N Spain). The study of the speleogenetic processes led to the identification of at least 6 paragenetic cave levels with associated sedimentary infill. In order to unravel the timing of changes in the karst dynamics and to get some insights about sediment origin, two sediment samples were collected from cave levels 4 and 1 for numerical dating purpose, using both Optically Stimulated Luminescence (OSL) and Electron Spin Resonance (ESR) methods. One additional modern-age sample was also taken from the entrance of the karst to evaluate the magnitude of the optical bleaching achieved by the quartz grains before entering the cave system. Last, one sample was collected from a flowstone for U-series dating, providing independent age control.OSL measurements were carried out using small quartz multi-grain (MG) and single-grain (SG) Single Aliquot Regenerative-dose (SAR) protocol. Initial Equivalent Dose (D_e) results show evidence of saturated OSL signal for the sample of the higher level (with ∼60% of saturated aliquots). Unlike SA data, SG analyses do not meet the usual quality criteria (e.g., relatively high recuperation ratios, only a few grains with useable signal), suggesting that corresponding dating results should be treated with caution.Hence, both MG and SG TT-OSL and MG ESR methods were subsequently employed, as the corresponding signals are known to have higher saturation levels than OSL ones. ESR analyses were based on the Multiple Centre (MC) approach using the standard multi-grain multi-aliquot additive (MAA) dose method, while TT-OSL measurements were performed following Demuro et al. (2020). The latter, however, did not return any useful results for both samples. MC ESR data show the usual D_e pattern (D_e(Al)>D_e(Ti op. D)>D_e(Ti–H)) indicating that among the three ESR signals analyzed, the Ti–H most likely provides the closest estimate to the true burial age. However, low measurement repeatability and goodness-of-of fit indicate that the reliability of the ESR results may be reasonably questioned.Results derived from this multi-technique dating approach provide the first chronological constraints for the sedimentary infill of the Alkerdi cave system. In particular, they suggest that sediment deposition in Cave Level 4 (ALK-OSL01) occurred around 130 ka, which is in good agreement with the minimum age constraint given by the speleothem (80.5 ± 9.0 ka). In comparison, the young age obtained for sample ALK-OSL02 (5.0 ± 0.9 ka) suggests recent Holocene formation of the lowest cave level 1.Finally, the MG De value obtained for the modern sample is close to zero (<1 Gy), indicating that the OSL signal is almost fully reset at a multi-grain level before entering the cave. Additionally, despite the large De overdispersion measured in this modern sample, the De values are one to two order of magnitude lower than those obtained with the same model in the other two samples. Therefore, the large OSL D_e overdispersion (OD) values of up to 64% obtained for the two samples from Cave Level 4 and 1 are most likely related to re-sedimentation processes inside the cave system.     

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.     

ESR chronology of the fluvial sequence of Cueva del Silo (Sierra de Atapuerca,Spain)

The Cueva del Silo is part of the lower karst level of the Cueva Mayor-Cueva del Silo karst system (Sierra de Atapuerca, Burgos, Spain), whose evolution has preserved an impressive archeo-paleoanthropological sequence since the Early Pleistocene. Cueva del Silo is remarkable for the presence of fluvial deposits that record the entry of the Arlanzón River water in the cave system, providing a key sequence to investigate the fluvio-karstic relationships that give rise to this endokarst system. In order to provide a chronological framework to these fluvial deposits, six sediment samples were dated by Electron Spin Resonance and 16 samples by paleomagnetism, collected from two outcrops: Galería de las Arenas and Sala del Caos. Our results provide maximum mean age of around 1600 ka and a minimum age of 916 ± 136 ka for the deposits in Sala del Caos. The younger date from Sala del Caos might represent the last fluvial input from Arlanzón River in the lower karst level. In contrast, ESR ages estimates of 1268 ± 133 ka and 1262 ± 108 ka were obtained for Galería de las Arenas sequence, which could indicate re-sedimentation processes from the intermediate karst level where similar ages were published. The annual dose might be wrongly assessed due to the re-sedimentation processes inside the karst, hence, ESR ages for these facies should be treated with extreme caution.     

On the interest of using the multiple center approach in ESR dating of optically bleached quartz grains: Some examples from the Early Pleistocene terraces of the Alcanadre River (Ebro basin,Spain)

The present work reports the first numerical ages obtained for the two highest fluvial terraces (Qt1 and Qt2) of the Alcanadre River system (Northeastern Spain) representing the earliest remnants of Quaternary morphosedimentary fluvial activity in the Ebro basin. ESR dating method was applied to optically bleached quartz grains and both the Al and Ti centers were measured, in accordance with the Multiple Center approach. The results are overall in good agreement with the existing preliminary chronostratigraphic framework and our interpretation indicate that terraces Qt1 and Qt2 have an ESR age of 1276 ± 104 ka and 817 ± 68 ka, respectively. These data provide some chronological insights on the beginning of the fluvial sedimentary processes in a scenario of incision maintained over Quaternary in the Ebro Basin. These are among the first numerical ages obtained for such high terraces in the Iberian Peninsula.Our results demonstrate the interest of using the Multiple Center approach in ESR dating of quartz, since the two centers provide complementary information, i.e. an independent dose control. The overall apparent consistency between the ESR age estimates and the existing preliminary chronostratigraphic framework may be considered as an empirical evidence that the Ti–Li center may actually work for Early Pleistocene deposits, whereas the Ti–H center shows some clear limitations instead. Finally, these results demonstrate the interest of using ESR method to date Early Pleistocene fluvial terraces that are usually beyond the time range covered by the OSL dating method.     

ESR dating of glacial moraine deposits: Some insights about the resetting of the germanium (Ge) signal measured in quartz

The electron spin resonance (ESR) dating of tills using germanium-doped (Ge) paramagnetic centers in quartz has advantages over other dating techniques, as quartz is common, processing is easy, and the technique has the potential for dating features several hundreds of thousands years old. ESR dating of moraines is based on the supposition that either subglacial comminution or exposure to sunlight resets the signal. However, actual dating suggests that a signal that is initially present cannot be bleached to zero by grinding alone. We found that grinding coarse samples (0.5–1 mm in diameter) to the mean grain size of fine sand (0.125–0.193 mm) reduced the signal intensity to 53–69% of its original value. From the value of the signal difference, one can devise a correction factor for ESR ages of subglacial sediment. Polymineralic grains are commonly present in till. Exposure of them to sunlight for several days can reduce the signal intensity to 7–8% of its original value within 1–2 mm thick of the sediment surface. However, within 5–8 mm of the sediment surface, exposure to sunlight for over one week only reduced the signal intensity to mean plateau values of 42–50% of the initial value. Mixing upper and lower layers of the samples during exposure to sunlight changed the signal intensity. This suggests that the amount of bleaching varies spatially. Sediments initially deposited at the margins of ice caps or ice sheets and subsequently overridden may have been sufficiently exposed to sunlight to allow ESR dating of moraines. The purity of the quartz and the grain size have significant impacts on signal intensity; intensive purification and the use of a uniform fine sand fraction are thus recommended.     

A Bayesian hierarchical age model for optical dating of single grains of quartz

In optical dating, the last time that a sample of sediment was exposed to sunlight is determined by dividing its equivalent dose (D_e) by the dose rate. For single-grain dating, the sample D_e is based on the statistical analysis of the distribution of D_e values estimated for individual grains, whereas the dose rate is usually determined from measurements of the environmental radioactivity of the bulk sample, together with allowances for radiation sources internal to the grains and cosmic rays. Conventionally, the D_e and dose rate are measured and analysed separately to produce an estimate of the depositional age of a sample, but this approach may result in loss of information because distributions of single-grain D_e values are influenced by several factors. Existing statistical models do not incorporate all the key information contributing to age estimation, such as the pattern and scale of dispersion of single-grain D_e values and dose rates, the associated measurement uncertainties, the effect of natural variability among grains, and the outlier probabilities of D_e and dose rate estimates. Here we propose an empirical Bayesian hierarchical age model (BHAM) for optical dating of quartz samples that incorporates the above information to estimate their depositional ages. The BHAM is based on the implementation of standardised growth curve and L_nT_n methods to integrate information on the full distribution of single-grain D_e values, sources of measurement uncertainty, beta-dose heterogeneity (observed or modelled), and detection of outliers. We present the results of validation tests using data sets of optically stimulated luminescence measurements and dose rates obtained for quartz samples dated previously from Denisova Cave (Russia) and for simulated samples. We conclude that the BHAM represents a robust and flexible approach to dealing with data for single grains of quartz within a Bayesian hierarchical framework and is suitable for application to sediments deposited in a variety of depositional settings.     

Chronology of an oyster reef on the coast of Bohai Bay, China: Constraints from optical dating using different luminescence signals from fine quartz and polymineral fine grains of coastal sediments

Fossil oyster reefs are indicators of past sea levels, and their formation is usually dated by means of radiocarbon. However, radiocarbon dating of the shells from coastal areas may be complicated by the varying sources of carbon. Here we applied optical dating methods to date the samples from above and below a fossil oyster bed in a section on the coast of Bohai Bay, China. The optical ages of the sediments were used to constrain the oyster bed. Single-aliquot regenerative-dose procedures using the OSL signal from fine grain quartz, the IRSL and post-IR OSL signals from polymineral fine grains were employed to determine equivalent dose (D_e). The behaviors of the different luminescence signals from quartz and polymineral grains during D_e measurements were examined. The results showed that the quartz OSL signal is more reliable than the polymineral IRSL and post-IR OSL signals with respect to dating for these coastal samples. The optical ages indicated that the oyster reef formed between ca. 6.2 and 5.0 ka.     

ESR dating of fluvial quartz: Estimate of the minimal distance transport required for getting a maximum optical bleaching

An ESR experimental study of artificial optical bleaching of sedimentary quartz has shown that the aluminum center was maximally bleached after a 6-month illumination equivalent to natural light. This duration seems too long to apply in natural conditions. Nevertheless, the measurement of the ESR intensity of aluminum centers in quartz extracted from modern sediments and deposited in sandy bars shows that the maximum bleaching has effectively been reached.

In order to determine the relationship between the bleaching and the distance covered by a quartz grain in a river, samples were collected along the Creuse River (France) from its spring to about 170 km downstream, where maximum bleaching levels were observed in previous studies. The ESR intensities of the aluminum and titanium centers in quartz were measured, using X-band spectroscopy, before and after artificial bleaching. The difference measured between these sub-samples shows that the maximum bleaching level is obtained in the course of the first kilometer. Hence, the assumption that ESR dating of fluvial sediment is based on the optical bleaching was validated.     

ESR dating of optically bleached quartz grains from Plio-Pleistocene to Holocene coastal dune deposits (Wilderness-Knysna area,South Africa): a comparison with luminescence

Five Plio-Pleistocene to Holocene aeolian quartz samples from the coastal dune deposits of the Wilderness-Knysna area (South Africa) previously dated by OSL were selected for ESR dating. Samples were processed following the Multiple Centre approach and using the Multiple Aliquot Additive dose method. Aluminium (Al) and Titanium (Ti) signals were systematically measured in all samples.Our study shows that ESR results obtained for Middle Pleistocene to Holocene samples may be strongly impacted by (i) the presence of a significant high frequency noise in the ESR spectra acquired for the Ti signals and (ii) the choice of the fitting function employed. In particular, if not taken into account, very noisy spectra can lead to a significant overestimation of the true ESR intensity measured for the Ti–H signal. These sources of uncertainty are however not sufficient to remove the ESR age overestimations. Consequently, our results indicate that the Al and Ti ESR signals of these quartz samples have not been fully reset during their aeolian transport.While this work contributes to improve our understanding of the ESR method applied to quartz grains, and especially of the potential and limitations of the Ti signals, it also provides additional baseline data to illustrate the existing variability among quartz samples of different origins or sedimentary context. Our results are consistent with previous studies by confirming that the Ti–H signal shows the best potential for the evaluation of low dose values (<100 Gy for these samples), whereas it becomes inappropriate for the higher dose range, and the Ti–Li–H (option D sensu Duval and Guilarte, 2015) should be used instead.Beyond the methodological outcome, this ESR dating study also provides a useful addition to the existing chronology of the aeolian deposits in this region. In particular, new (and possibly) finite numerical age results were obtained for the two oldest samples, constraining the aeolianite landward barrier dune and the coversand formations to the MIS 10-8 and Pliocene, respectively.     

ESR dating of the Eupchon fault, South Korea

We investigated temporal pattern of Quaternary fault activity of the Eupchon fault zone in the southeastern part of the Korean peninsula, using ESR dating of fault rocks. The counterfeit E′ signal significantly affected the equivalent dose on some samples. In particular, the counterfeit E′ signal tends to affect samples with E′ intensity close to saturation level. Storage at room temperature for 360 days and heating at 170 °C for 15 min. after γ-ray irradiation did not change significantly the intensities, the dose responses and ESR ages for OHC, Al, and Ti signals. ESR ages from the Eupchon fault zone range from 2000 to 500 ka. The fault rocks were reactivated at least five times 2000, 1300, 900–1100, 700–800, and 500–600 ka ago. These data indicate that long-term cyclic fault activity of this fault zone continued into the Quaternary. The results from this study suggest that the Eupchon fault zone can be classified as a potentially active fault and presents some potential seismic hazards to the nuclear power plant in its vicinity.     

New ESR/U-series dates of the lowest Acheuleo-Yabrudian levels of Qesem cave

Qesem cave is a Middle Pleistocene site located close to Tel Aviv, Israel, assigned to the Acheuleo-Yabrudian Cultural Complex (AYCC) of the Lower Palaeolithic. The site provides rich assemblages of knapped flint, animal remains and some human teeth making it of particular interest. Its location in the Levantine corridor confers a major interest to the understanding of human dynamics during the Middle Pleistocene.A series of 6 herbivorous teeth from the base of the 11 m archaeological sequence of AYCC Qesem Cave was analysed by combined ESR/U-series method; this complements previous dating series carried out on teeth and on heated flints on higher parts of the sequence (Mercier et al., 2013; Falguères et al., 2016) The teeth were measured according a regular protocol for which each tissue was analysed by inductively coupled plasma-quadrupole mass spectrometry (ICP-Q-MS) for U-series using a combination of a Thermo iCAP-RQ mass spectrometer coupled to a Cetac Aridus III desolvator system, and ESR analyses were implemented on enamel tissue. All these data were combined in order to yield modelled ages.The goal was to find out whether there was a time gap between the carbonates layers dated to 420 ka (Gopher et al., 2010) and archaeological layers of the AYCC found throughout the cave's sequence. The new results yield ages ranging between 220 and 430 ka confirming a great antiquity and a long duration of AYCC in the Levant.     

Optical dating of Holocene lake sediments: Elimination of the feldspar component in fine silt quartz samples

Optically stimulated luminescence of fine silt quartz was investigated to establish chronologies for lake sediments from the British Isles. Feldspar contamination and its potential effects on equivalent dose (D_e) determination were examined. A new feldspar contamination test based on the thermal quenching of quartz OSL and thermal assistance of feldspar OSL identified feldspar contamination in samples being treated for 20 min in 20% hydrofluoric acid. Feldspar component monitoring based on the post-IR OSL/OSL ratio was not sufficiently sensitive to monitor a feldspar component, but is a good indicator whether a standard SAR procedure can be applied successfully, despite the presence of feldspar. Based on these results we used a modified SAR protocol including a 100 s IRSL stimulation at 50 °C before OSL readout. This protocol could overcome any malign effects of feldspar even for a feldspar bearing polymineral sub-sample.     

ESR/U-series chronology of the Lower Palaeolithic palaeoanthropological site of Visogliano, Trieste, Italy

The Visogliano shelter, in north-eastern Italy, is an important Middle Pleistocene occupation site where human remains were found together with an archaic lithic industry, including choppers, chopping tools and a few protobifaces. It is of utmost importance to try to document this period, when a second wave of settlement colonised Western Europe, carrying new flaking techniques and tools.Combined ESR/U-series analyses, integrated with biostratigraphical and environmental data, define a chronological frame for the layers from which the artefacts were unearthed. The lower levels, including human remains, can be dated to the 350–500 kyr time span, in agreement with micromammal and stratigraphical studies.These data make Visogliano one of the oldest palaeoanthropological sites in Italy, where human remains are directly associated with protobifaces, choppers and chopping tools. In Western Europe, Visogliano is contemporaneous to the G soil of the Arago Cave, France, with which it shares several similarities in faunal assemblages and radiometric data, and which contains human remains also. These data make Visogliano as one of the oldest sites in Europe where the Acheulian culture is observed.     

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.     

Exploring the potential of luminescence methods for dating Alpine rock glaciers

Rock glaciers contain valuable information about the spatial and temporal distribution of permafrost. The wide distribution of these landforms in high mountains promotes them as useful archives for the deciphering of the environmental conditions during their formation and evolution. However, age constraints are needed to unravel the palaeoclimatic context of rock glaciers, but numerical dating is difficult. Here, we present a case study assessing the potential of luminescence techniques (OSL, IRSL) to date the inner sand-rich layer of active rock glaciers. We focus on the signal properties and the resetting of the signal prior to deposition by investigating single grains. While most quartz shows low signal intensities and problematic luminescence characteristics, K-feldspar exhibits much brighter and well-performing signals. Most signals from plagioclases do not show suitable properties. Luminescence signals far below saturation indicate distinct but differential bleaching. The finite mixture model was used to determine the prominent populations in the equivalent dose distributions. The luminescence ages represent travel times of grains since incorporation into the rock glacier and hence, minimum ages of rock glacier formation. Luminescence ages between 3 ka and 8 ka for three rock glaciers from the Upper Engadine and Albula region (Swiss Alps) agree well with independent age estimates from relative and semi-quantitative approaches. Therefore, luminescence seems to have the potential of revealing age constraints about processes related to the formation of rock glaciers, but further investigations are required for solving some of the problems remaining and reducing the dating uncertainties.     

ESR and OSL dating of fossil-bearing deposits from Naracoorte Cave Complex palaeontological sites,south Australia

Little work has been undertaken on combined dating of sedimentary quartz grains using electron spin resonance (ESR) and optically stimulated luminescence (OSL) techniques in Australia. This study aims to assess the suitability of a combined ESR and OSL dating approach for establishing improved chronologies of Middle-Late Pleistocene deposits within the Naracoorte Cave Complex (NCC), South Australia. Here, we apply ESR and OSL dating in tandem to a series of samples collected from three different NCC sites: Whale Bone, Specimen and Alexandra cave. ESR quartz dating focuses on the multi-centre (MC) approach, which involves comparative evaluations of Al and Ti centre signals, while paired luminescence dating focuses on single-grain OSL analysis and includes examination of multi-grain averaging effects. The comparative ESR-OSL dating results exhibit broad agreement for deposits spanning 50–150 thousand years, with either the Ti–H or Al centre ages overlapping with paired OSL ages at 2σ in nearly all cases. MC ESR evaluations (Al v Ti–Li v Ti–H age assessments) indicate incomplete resetting of the bleachable Al centre signal for a small number of samples. Two-thirds of samples exhibit Ti–Li ages that are significantly older than corresponding Al centre ages, which is unexpected from a bleaching kinetics perspective and may indicate a broader reliability issue for Ti–Li palaeodose evaluation with these particular samples. Our findings: (i) support the applicability of both palaeodosimetric dating methods in this depositional setting; (ii) highlight the merits of applying combined ESR-OSL analyses in tandem, and; (iii) provide one of the first reliable evaluations of quartz ESR MC dating for samples with natural dose ranges as low as only a few tens of Gy. These results show that the Whale Bone, Specimen and Alexandra cave sites are temporally related and can be used to derive multi-site reconstructions of faunal assemblages and palaeoenvironmental history.     

New radiometric dates on the lowest stratigraphical section (TD1 to TD6) of Gran Dolina site (Atapuerca,Spain)

Ages based on independent methods, such as combined ESR-U series, luminescence, and magnetostratigraphic analyses have been obtained for the upper stratigraphical section of Gran Dolina site (TD6 to TD11 levels). However, the chronostratigraphical framework of this European Paleolithic key site remains incomplete because of its great antiquity and the lack of reliable methods. This paper provides new radiometric dates by electron spin resonance applied to optically bleached quartz grains for the whole stratigraphic sequence. The results agree with the previous chronostratigraphical framework for the upper part of the stratigraphical sequence. The ages for the Homo antecessor remains from TD6 layer range between 800 and 900 ka. The lowest layers attributed to endogenous sediments (TD1) could be contemporaneous with the Sima del Elefante TE9 human bearing layer dated to 1.2 Ma. The results suggest a human occupation of possibly more than 1 Ma at the Gran Dolina site. This study confirms moreover the potential of ESR dating method applied on quartz in karstic environment.     

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.     

Optically stimulated luminescence dating of loess in South-Eastern China using quartz and polymineral fine grains

Loess deposits distributed in southeastern China play an important role for paleoclimate reconstruction of the subtropical regions. These loess-paleosol deposits are mainly spread within the middle and lower reaches of the Yangtze River as well as in the drainage area of the Huai River. The ages of loess paleosol sequences that are distributed along the Huai River are not well constrained. In this study, the standard single-aliquot regenerative dose (SAR) optically stimulated luminescence (OSL) protocol and two elevated temperature post infrared-infrared stimulated luminescence SAR protocols (pIRIR₂₂₅ and pIRIR₂₉₀) were applied on 4–11 μm quartz and polymineral fine grains, respectively, in order to obtain the first numerical luminescence chronology for a loess-paleosol sequence in northern Jiangsu Province. Our results show a good agreement between quartz SAR-OSL and polymineral pIRIR ages up to ~70 ka. These findings confirm that Xiashu loess accumulated during the Last Glaciation. For samples older than this, the ages increasingly deviate with depth. Fine quartz ages beyond 70 ka are interpreted as underestimates, as previous studies reported that quartz ages >70 ka from various sedimentary origins worldwide may underestimate even if they pass rejection criteria and dose recovery tests. On the other hand, the pIRIR ages are most likely overestimating the true depositional ages as indicated by the results of dose recovery tests, where a 30–60% overestimation of the recovered dose is reported for values larger than ~400 Gy. The overestimation of pIRIR protocols was also confirmed by the results obtained when large beta doses were added on top of the natural accrued dose. Moreover, our dating results suggest that L1/S1 transition (corresponding to MIS 5/4 boundary) occurred much higher in the stratigraphic sequence than may have been interpreted from the magnetic susceptibility enhancement. This inconsistency can be assigned to invalidity of magnetic susceptibility as a chronostratigraphical proxy due to ferrimagnetic minerals dissolution or transformation during paedogenesis processes in this humid subtropical region in the southeastern China.