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.     

Age of the oldest hominin settlements in Spain: Contribution of the combined U-series/ESR dating method applied to fossil teeth

This paper presents a synthesis of the combined Uranium-Series/ESR age results obtained on fossil teeth from several Early Pleistocene archaeological and/or palaeontological Spanish localities: Atapuerca Gran Dolina TD-6, Fuente Nueva-3, Barranco León, Venta Micena and Vallparadís. While the age results show some scattering, they are nevertheless encouraging and provide a significant contribution to the understanding of the first hominin settlements in Western Europe.These “old” samples are mainly characterised by high ²³⁰Th/²³⁴U activity ratios that may sometimes exceed secular equilibrium, and by high Uranium concentrations (several tens of ppm or more). The modelling of U-uptake is therefore really crucial for the age calculation process. In the case of the combined US–ESR approach, this uptake is derived from the U-series data measured in dental tissues, which seem to be strongly dependant on the hydro-geological context. Consequently, when dating “old” samples, a special attention has to be paid to the accuracy and the meaning of the U-series data collected from the dental tissues, which may be influenced by several factors such as spatial heterogeneity and recent U-uptake overprint. Some rapid scanning procedures should be developed in order to pre-identify the samples that are the most suitable for ESR dating.     

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.     

ESR chronology of alluvial deposits in the Arlanzón valley (Atapuerca,Spain): Contemporaneity with Atapuerca Gran Dolina site

The Sierra de Atapuerca (Northern Spain) is characterized by a well-developed karst system where several major archaeological sites have been discovered, attesting an almost continuous hominin occupation of the area during the whole Pleistocene period. Previous geomorphological studies showed a connection between genesis of the karst system and the evolution of the nearby Arlanzón river Valley. However, numerical dating results were missing to refine the chronostratigraphical framework of the Arlanzón valley's fluvial incision. To address this, we applied the Electron Spin Resonance (ESR) dating method to sedimentary optically bleached quartz grains from several fluvial terraces. Nine samples were collected from five of the 14 identified terraces. The ESR age results are stratigraphically coherent and in general agreement with both previous geomorphological observations and available palaeomagnetic data. Consequently, an ESR chronology of the geological evolution of the Arlanzón valley is proposed, which can be then correlated to the sedimentary sequence of the palaeoanthropological site of Atapuerca Gran Dolina. Our results provide important information about the chronology of hominid occupation in this area during Early and Middle Pleistocene.     

Uplift rates defined by U-series and 14C ages of serpulid-encrusted speleothems from submerged caves near Siracusa,Sicily (Italy)

We have established a plausible rate of uplift near Siracusa in southeastern Sicily (Italy) over the last glacial–interglacial cycle using U-series ages of submerged speleothem calcite and ¹⁴C ages of calcite serpulid layers that encrust the speleothems during cave submergence. The precisely determined ages of these sea level benchmarks were compared with expected relative sea level position based on glacio-hydro-isostatic modeling to assess the rate of uplift in this region. When combined with the age of various late Holocene archaeological sites that have been recently described and characterized in terms of their functional position relative to sea level these data collectively define a rate of uplift ≤0.4 mm a^?1 along this portion of the Sicilian coastline. These results are consistent with an age assignment of marine isotope stage (MIS) 5.3 or 5.5 for the Akradina terrace, which in turn places temporal constraints on paleoshorelines above and below this level.     

Chronology of the Upper Pleistocene loess sequence of Havrincourt (France) and associated Palaeolithic occupations: A Bayesian approach from pedostratigraphy,OSL, radiocarbon,TL and ESR/U-series data

In connection with the future Seine-North Europe Canal (Seine-Scheldt), a large-scale rescue archaeological survey was conducted at Havrincourt (northern France) between 2008 and 2011. The discovery of several levels of Palaeolithic flint artefacts embedded in a relatively thick loess sequence (ca 6–7 m) preserved on a gentle slope facing North-East, resulted in a 6000 m² excavation. This opened the opportunity for a detailed pedosedimentary and interdisciplinary geochronological survey (¹⁴C, optically stimulated luminescence, thermoluminescence, ESR/U-series) that has allowed us date the sequence reliably. On the basis of these results we propose this sequence as a new pedostratigraphic and archaeological reference sequence for northern France. We present here the optical dating of the sequence performed on fine (4–11 μm) quartz grains extracted from 17 samples. The luminescence characteristics of these extracts indicate that the single-aliquot regenerative dose optically stimulated luminescence (SAR-OSL) procedure that was applied is well suited. A consistent set of optical ages was obtained for the loess deposited up to around 70 ka ago. Independent age control (pedostratigraphy, ¹⁴C, ESR/U-series dates) allowed us to apply a Bayesian approach to build a chronometric model. This in turn enabled a regional chronostratigraphic framework to be built, to constrain the correlations with neighboring regions (northern France and Belgium) and to calculate a precise age for the four Palaeolithic levels discovered, including a unique occupation related to the early Upper Palaeolithic which was previously unknown in the area.     

New Th-U and C age determinations from Piton des Neiges volcano, Reunion — A revised chronology for the Differentiated Series

²³⁰Th-²³⁸U age measurements were carried out on 18 samples of lava from Piton des Neiges. These lavas range from basalts to trachytes. The ages extend from 270,000 to 12,000 a B.P. and cover most of the period in which Differentiated Series magmas were erupted. New ¹⁴C ages on charcoal sampled in young pyroclastic deposits are also presented. The late-stage evolution of the volcano is discussed in the light of these new ages and a chronology of the explosive activity is given. The oldest pyroclastic flow (Ste. Suzanne) is more than 220,000 a; other pyroclastic units were emitted between 220,000 and 110,000 a. There were at least two episodes of caldera formation: the first episode is inferred to have occurred about 190,000 a ago; the last occurred between 190,000 and 110,000 a. Although the most recent lava activity was mainly concentrated on the eastern flank of the volcano and around the summit area, it also occurred, about 70,000 a ago, in the southwestern part of the massif. The youngest explosive activity (about 50,000 to 20,000 a) on the eastern flank of the volcano has now been dated by three different methods (¹⁴C and Th-U ages on block- and ash-flow tuffs, K-Ar ages on associated domes). Youthful explosive activity (about 35,000 to 12,000 a) on the western flank of the volcano is also demonstrated by ¹⁴C dating on charcoal and by a Th-U age of 12,000 a on a trachytic nuée ardente deposit. This last age indicates that activity may have persisted later than previously supposed and implies a high rate of erosion for the Cirque de Mafate.     

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 chronology of alluvial deposits and first human settlements of the Middle Loire Basin (Region Centre,France)

Since 1970, many prehistoric sites have been discovered in the alluvial terraces of several rivers of the Middle Loire River basin (France). During the last decade, the stepped-terraces systems of three of the Loire tributaries, the Creuse, the Cher and the Loir Rivers, were the focus of multidisciplinary studies, involving Quaternary geology, prehistory and geochronology. The geochronological data now available for these systems were mainly obtained by electron spin resonance (ESR) method applied to optically bleached fluvial quartz. These results provide a chronological framework for the evolution of fluvial systems and the human settlements of this area during Lower and Middle Pleistocene. Two phases of human settlement could be distinguished, around 1.1 Ma (Early Palaeolithic – Mode 1) and around 0.7 Ma ago (Acheulean – Mode II).     

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 and ESR/U-series dating study of several middle Palaeolithic sites of Pléneuf-Val-André (Brittany,France): Piégu,Les Vallées and Nantois

The area of Pléneuf-Val-André, Brittany, France, has delivered several Palaeolithic sites containing palaeontological remains, very rare into this granitic area. In order to precise the stratigraphical framework of the prehistoric human occupations of this zone, an ESR dating program was initiated in the late 1980s and different kinds of materials (mammal bones and teeth, naturally bleached quartz extracted from marine or aeolian sediments and marine mollusc shells) were then sampled for geochronological analyses. The present paper displays the main obtained results on three stratigraphically connected middle Palaeolithic sites: Piégu, Les Vallées and Nantois. The results are consistent with the regional chronostratigraphic framework and permit to suggest palaeoenvironmental reconstruction of the area and the dating of the various archaeological evidences.     

Depth-dependence of the production rate of in situ 14C in quartz from the Leymon High core,Spain

To constrain the depth-dependence of in situ ¹⁴C production we measured the cosmogenic ¹⁴C concentration of quartz separates along a quartzite core from the Leymon High site in northwest Spain. A total of 16 quartz samples were measured over a depth range of 1–1545 cm (3–4017 g cm⁻²). The obtained ¹⁴C profile was modeled using a neutron production rate, exponentially decreasing with depth, and a fast and negative muon production parameterized as a function of the local muon flux as derived by (Heisinger et al., 2002a, 2002b). This model yields a total negative muon capture probability of 1.72 (+0.22/−0.56) × 10⁻² and a fast muon reaction cross section of 0 (+11.8/−0.00) μb. Rescaled to sea level high latitude using a Lal/Stone scaling scheme, these estimates yield a surface muon production rate of 3.31 (+0.43/−1.07) and 0 (+0.42/−0.00) at·g⁻¹ yr⁻¹ for negative muon capture and fast muons, respectively. This is the first muon production estimate for in situ ¹⁴C from a natural setting and is within uncertainty of the previous experimental estimates. The present contribution also provides new long-term blank and standard (PP-4, CRONUS-A & CRONUS-N) in situ ¹⁴C data from the ETH Zürich ¹⁴C extraction line.     

OSL and ESR studies of Aeolian quartz from the Upper Pleistocene loess sequence of Nussloch (Germany)

As part of a chronological study of the famous Upper Pleistocene Nussloch (Germany) loess sequence, three samples were collected to check the applicability of palaeodosimetric dating methods (OSL and ESR) to quartz grains. The ESR-multicentre method showed a partial bleaching of the ESR centers in aeolian sands. This partial bleaching was also observed by OSL. Laminated loess seemed to be sufficiently bleached but showed a large scatter of the doses, which we ascribed to heterogeneous responses of the luminescent grains to the SAR protocol. Ages could nevertheless be calculated for the three samples and were found to be somewhat older than the IRSL and ¹⁴C ages obtained for the same layers of the laminated loess.     

New fossil eccoptarthrids (Coleoptera: Curculionoidea) from the Yixian Formation of western Liaoning, China

One new genus and three new species of the weevil family Eccoptarthridae (Curculionoidea), Leptocar polychaetus gen. et sp. nov., Abrocar macilentus sp. nov., Cretonanophyes punctatus sp. nov., are described and illustrated. They pertain to the Upper Jurassic or Lower Cretaceous Yixian Formation of western Liaoning Province, China. The host plants to the living eccoptarthrids and the floras in Yixian Formation indicate that those archaic eccoptarthrids possibly lived on conifers with a phylogenetic closeness to Cupressaceae. Besides, the early diversification of eccoptarthrids is discussed: origi- nated in Central or East Asia in the Late Jurassic, spread into Western Europe and South America during the Early Cretaceous, underwent a dramatic decline after the Early Cretaceous which likely was caused by competitive pressure and the displacement of their host plants.     

Chronology of Upper Pleistocene sequences at Sidi Messaoud (wadi Noun, southwestern Morocco) based on C, optical and U-series dating

The Sidi Messaoud site provides a 40 m thick sedimentary infilling of great importance for the study of environmental changes and landscape evolution during the Upper Pleistocene in the Western Sahara. In this study, chronological results obtained by the ¹⁴C, U-series and optical dating techniques are compared. Each individual age, depositional environment and post-deposition history of the various samples are evaluated, in order to explain the methodological reasons for discordances and concordances. Stratigraphic and palaeoenvironmental implications for the last 120 ka history in southwestern Morocco are also inferred: the wadi Noun gorges had been incised before MIS 5, and later, during MIS 3, the valley has been filled in with a mean sedimentation rate of 1 m/ka.     

Counting chronology and climate records with about 1000 annual layers of a Holocene stalagmite from the Water Cave in Liaoning Province, Chinaannual layers of a Holocene stalagmite from the Water Cave in Liaoning Province, China

One active stalagmite from the Water Cave in Liaoning Province contains growth layers of three sizes. Based on thermal ionization mass spectrometry ²³⁰Th dating, we found that middle size layers are annual layers, with each middle layer consisting of one narrow dark layer and a wide bright layer. The small layers within middle layers are sub-annual layers and the large layers are multi-year layers. Based on the layer-counting method, we established a high-resolution time scale for layer thickness. Our results reveal two dramatic century-scale climate cycles over the past 1000 years in this region.     

Counting chronology and climate records with about 1000 annual layers of a Holocene stalagmite from the Water Cave in Liaoning Province, China

One active stalagmite from the Water Cave in Liaoning Province contains growth layers of three sizes. Based on thermal ionization mass spectrometry 230Th dating, we found that middle size layers are annual layers, with each middle layer consisting of one narrow dark layer and a wide bright layer. The small layers within middle layers are sub-annual layers and the large layers are multi-year layers. Based on the layer-counting method, we established a high-resolution time scale for layer thickness. Our results reveal two dramatic century-scale climate cycles over the past 1000 years in this region.     

A new fossil kentriodontid dolphin (Cetacea; Kentriodontidae) from the Middle Miocene Takinoue Formation, Hokkaido, Japan

Abstract Kentriodon hobetsu , a new species, is described from a partial skull from the Middle Miocene Takinoue Formation, in Hokkaido, Japan. The holotype skull includes the base of the rostrum and a fairly well preserved braincase. The new species is distinguished clearly from previously described species of Kentriodon Kellogg, 1927, by the shape of the anterior margin of the pterygoid sinus fossa, the large premaxilla, rounded facial margin, and lesser development of rugosities and processes. This new record of Kentriodon , the first named kentriodontid dolphin from the western North Pacific, extends the geographic range of the genus significantly.     

Underestimated ~(14)C-based chronology of late Pleistocene high lake-level events over the Tibetan Plateau and adjacent areas: Evidence from the Qaidam Basin and Tengger Desert

The palaeolake evolution across the Tibetan Plateau and adjacent areas has been extensively studied, but the timing of late Pleistocene lake highstands remains controversial. Robust dating of lacustrine deposits is of importance in resolving this issue. This paper presents 14 C or optically stimulated luminescence(OSL) age estimates from two sets of late Quaternary lacustrine sequences in the Qaidam Basin and Tengger Desert(northeastern Tibetan Plateau). The updated dating results show:(1) the radiocarbon dating technique apparently underestimated the age of the strata of >30 ka BP in Qaidam Basin;(2) although OSL and 14 C dating agreed with each other for Holocene age samples in the Tengger Desert area, there was a significant offset in dating results of sediments older than ~30 ka BP, largely resulting from radiocarbon dating underestimation;(3) both cases imply that most of the published radiocarbon ages(e.g., older than ~30 ka BP) should be treated with caution and perhaps its geological implication should be revaluated; and(4) the high lake events on the Tibetan Plateau and adjacent areas, traditionally assigned to MIS 3a based on 14 C dating, are likely older than ~80 ka based on OSL chronology.     

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.