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.     

Electron spin resonance dating of quartz from archaeological sites at Victoria Falls,Zambia

When electron spin resonance (ESR) is applied to sedimentary quartz, dealing with the poor bleachability of the signals is particularly challenging. In this study, we used both the single-grain optically stimulated luminescence (OSL) and the single aliquot ESR dating of quartz from deep sand deposits preserving a Stone Age archaeological sequence to combine the advantages of the two methods: good bleaching behaviour and extended age range. Using the youngest samples at each sampling site we were able to calculate the mean ESR residual age from the difference between the OSL ages and the apparent ESR ages. Focusing mainly on the single aliquot regenerative dose (SAR) protocol here, we were able to calculate the mean ESR residual age for the Ti and Al centres, including the non-bleachable signal component for the latter. For the NP site, residual ages of 209 ± 13 ka and 695 ± 23 ka were calculated for the two centres, whereas for the ZS site 268 ± 39 ka and 742 ± 118 ka were determined. These residual ages are significant and cannot be neglected. Thus, the residual age was subtracted from the apparent ESR ages. The validity of the residual subtraction method was tested through a comparison of the oldest OSL age from each site with the residual subtracted ESR age. For both NP and ZS sites, the residual subtracted Ti and Al ages were consistent with the OSL age within 2-σ uncertainty, and therefore confirm the robustness of the subtraction method. Within the NP sequence, we were able to locate the end of the Early Stone Age at 590 ± 86 ka, and this provides a maximum age for the transition to the Middle Stone Age in this part of south-central Africa.     

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).     

From mass‐wasting to slope stabilization – putting constrains on a tectonically induced transition in slope erosion mode: a case study in the Judea Hills,Israel

Calcrete‐coated remnants of landslide debris and alluvial deposits are exposed along the presently stable hillslopes of the Soreq drainage, Judea Hills, Israel. These remnants indicate that a transition from landslide‐dominated terrain to dissolution‐controlled hillslope erosion had occurred. This transition possibly occurred due to the significant decrease in tectonic uplift during the late Cenozoic. The study area is characterized by sub‐humid Mediterranean climate. The drainage hillslopes are typically mantled by thick calcrete crusts overlying Upper Cretaceous marine carbonate rocks. Using TT‐OSL dating of aeolian quartz grains incorporated in the calcrete which cements an ancient landslide deposit, we conclude that incision of ~100 m occurred from 1056 ± 262 to 688 ± 86 ka due to ~0·3° westward tilt of the region; such incision invoked high frequency of landslide activity in the drainage. The ages of a younger landslide remnant, alluvial terrace, and alluvial fan, all situated only a few meters above the present level of the active streambed, range between 688 ± 86 ka and 244 ± 25 ka and indicate that since 688 ± 86 the Soreq base level had stabilized and that landslide activity decreased significantly by the middle Pleistocene. Copyright © 2012 John Wiley & Sons, Ltd.     

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.     

A multi-method approach to dating middle and late Quaternary high relative sea-level events on NW Svalbard – A case study

Waxing and waning ice sheets and changing sea levels have been interpreted from the Quaternary stratigraphic record at Leinstranda, Brøggerhalvøya in NW Svalbard. We have identified seven high relative sea-level events, related to glacio-isostatic loading, and separated by at least four glacial events. To establish a chronology for the high sea-level events (interstadials and interglacials) and the intervening glaciations, we have used three different absolute dating methods: optically stimulated luminescence (OSL) of shallow marine deposits, and electron spin resonance (ESR) and radiocarbon (AMS-¹⁴C) dating of fossils contained in these sediments. Of the absolute dating methods, OSL has provided the stratigraphically most consistent dataset and which also matches a biostratigraphically inferred interglacial. The ESR ages of mollusc shells suffer from low precision due to unusually large uranium content in most dated shell samples, which in turn is most likely a result of significant recent uranium enrichment of the sediments. Most radiocarbon ages are non-finite. The results show that the high relative sea-level events range in age from the Saalian sensu lato (≥Marine Isotope Stage, MIS, 6) to the early Holocene (MIS 1), and include events OSL-dated to 185 ± 8 ka, 129 ± 10 ka, 99 ± 8 ka and 36 ± 3 ka. The methods used by us and by previous investigators of the same site are compared and assessed, and sources of error, accuracy and precision of ages are discussed.     

Ages of Liangshan Paleolithic sites in Hanzhong Basin,central China

Thermally transferred optically stimulated luminescence (TT-OSL) dating extends the age range beyond current limits of OSL dating in Chinese loess. In this study, we use a single-aliquot regenerative-dose procedure for TT-OSL protocol to date Yaochangwan and Hejialiang localities of loess-covered Liangshan Paleolithic sites in Hanzhong Basin, which is an important area for the study of Paleolithic industries during the middle Pleistocene in central China. The results suggest that buried culture layer at the Hejialiang locality is correlated with the last interglacial paleosol S1 in Chinese Loess Plateau, it is dated at 86.3 ± 6.4 ka. The Yaochangwan locality spans from approximate 600–100 ka and correlates with S5–S1 in the typical Chinese loess–paleosol sequences, respectively. These ages suggest that hominins already occupied the Hanzhong Basin since approximately 600 ka ago.     

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.     

Surface exposure dating of Holocene basalt flows and cinder cones in the Kula volcanic field (Western Turkey) using cosmogenic 3He and 10Be

The Kula volcanic field in Western Turkey comprises about 80 cinder cones and associated basaltic lava flows of Quaternary age. Based on geomorphological criteria and K-Ar dating, three eruption phases, β2–β4, were distinguished in previous studies. Human footprints in ash deposits document that the early inhabitants of Anatolia were affected by the volcanic eruptions, but the age of the footprints has been poorly constrained. Here we use ³He and ¹⁰Be exposure dating of olivine phenocrysts and quartz-bearing xenoliths to determine the age of the youngest lava flows and cinder cones. In the western part of the volcanic field, two basalt samples from a 15-km-long block lava flow yielded ³He ages of 1.5 ± 0.3 ka and 2.5 ± 0.4 ka, respectively, with the latter being in good agreement with a ¹⁰Be age of 2.4 ± 0.3 ka for an augen gneiss xenolith from the same flow. A few kilometers farther north, a metasedimentary xenolith from the top of the cinder cone Çakallar Tepe gave a ¹⁰Be age of 11.2 ± 1.1 ka, which dates the last eruption of this cone and also the human footprints in the related ash deposits. In the center of the volcanic field, a basalt sample and a metasedimentary xenolith from another cinder cone gave consistent ³He and ¹⁰Be ages of 2.6 ± 0.4 ka and 2.6 ± 0.3 ka, respectively. Two β4 lava flows in the central and eastern part of the volcanic province yielded ³He ages of 3.3 ± 0.4 ka and 0.9 ± 0.2 ka, respectively. Finally, a relatively well-preserved β3 flow gave a ³He age of ∼13 ka. Taken together, our results demonstrate that the penultimate eruption phase β3 in the Kula volcanic field continued until ∼11 ka, whereas the youngest phase β4 started less than four thousand years ago and may continue in the future.     

Age comparison by luminescence using quartz and feldspar on core HPQK01 from the Pearl River delta in China

Reliable chronology is critical for reconstructing estuarine delta process. In this study, detailed chronological framework has been performed on a core HPQK01 (52 m in depth) from the central Pearl River delta (PRD) of China. Both quartz OSL and feldspar post-IR IRSL (pIRIR) methods for late Pleistocene sediments, as well as radiocarbon dating for Holocene sediments, were applied to date the core. Results show that quartz OSL ages range from 125 ± 18 ka to 58 ± 6 ka, and that all of them were minimum ages due to the OSL signal saturation. Feldspar pIR₂₀₀IR₂₉₀ protocol shows some overestimation in dose recovery test, with the recovered to the given ratio of 1.2, while a ratio of around 1 was obtained for feldspar pIR₅₀IR₂₅₀ signals. Robust ages have been obtained from feldspar fading corrected pIR₅₀IR₂₅₀ dating with ages ranging from 150 ± 17 ka to 98 ± 12 ka. AMS ¹⁴C results suggest that subtidal-intertidal zone was deposited during the middle Holocene from 8.21 ± 0.19 cal ka BP to 4.99 ± 0.25 cal ka BP. The sedimentology of core HPQK01 record two marine transgressive-regressive cycles. Based on the dating results, the lower fluvial sediment unit (T2) could be correlated to marine isotope stage (MIS) 6, and the lower marine unit (M2) was deposited during MIS 5. A sedimentary hiatus occurred with age range of from MIS 4 to MIS 2. Since middle Holocene, another marine stratum (M1) has been accumulated. Overall, our findings suggest that feldspar pIRIR dating method has the potential to establish the Quaternary chronostratigraphic framework of the PRD for samples with ages within 150 ka.     

Evaluating OSL-SAR protocols for dating quartz grains from the loess in Ili Basin,Central Asia

Late Pleistocene records of loess deposition are a critical archive for understanding terrestrial paleoenvironment changes in Central Asia. The age of loess is not well known for the deserts regions and surrounding high plateaus in Central Asia. Previous studies have shown that there remains a disparity between ages for loess deposition by luminescence and ¹⁴C dating. This study evaluates the potential of optically stimulated luminescence (OSL) to date a loess sequence resting on fluvial sands in the east Ili Basin, Central Asia. The single-aliquot regenerative-dose (SAR) protocol on coarse grain quartz was employed for equivalent dose determinations. The basal fluvial sand returned a secure OSL age, with low overdispersion value in equivalent doses (19 ± 2%) of ca. 36 ka and provides a close, but maximum age estimate (within 5 ka) on the initiation of loess deposition. However, the loess yielded high overdispersion values for equivalent doses and age reversals, coincident with diffuse paleosols; indicating that pedoturbation with loess deposition may be a dominant process. OSL ages between ca. 45 and 14 ka calculated using a maximum age model and OSL ages from other sites in the Basin suggests that the latest major period of loess deposition was between 70 and 10 ka ago. A future hypothesis to test based on these analyses is that there may be three periods of heightened loess deposition at ca. 45, 35 to 19 and 14 ka, when desert source areas to the west were particularly dry.     

嫩江断裂带北段的第四纪活动特征初步研究

嫩江断裂带是松辽盆地的西边界断裂,但受第四系强覆盖等研究条件的限制,前人对该断裂第四纪构造活动的研究较少。本文针对该断裂带北段开展了野外地质调查,并综合大地电磁测深和纵波速度结构等结果,初步研究了嫩江断裂带北段的第四纪活动特征。调查发现,该断裂北段主要发育地貌陡坎、基岩滑坡、地层揉皱变形、近垂直擦痕、基岩崩塌与线性断塞塘等特征。探槽古地震研究揭示断裂带北段在（80.9±4.6）—（62.9±2.3）ka BP曾发生1次古地震事件,运动方式为正断,垂直位移量约1.5m,震级约为M_S 7.1—7.3,断裂在晚更新世曾发生过强烈活动。研究结果有助于认识了解该断裂和松辽盆地的第四纪构造变形过程,并为评价该断裂及邻区的地震活动潜势提供参考。     

Lavini di Marco (Trentino,Italy): 36Cl exposure dating of a polyphase rock avalanche

The Lavini di Marco rock avalanche deposit (“Marocca di Marco”) is located along the left side of the middle Adige Valley, south of the town of Rovereto (NE Italy). The deposit is estimated to have a volume of ∼2 × 10⁸ m³ and cover an area of ∼6.8 km². It comprises Jurassic Calcari Grigi limestones that detached from the western slope of Mt. Zugna Torta. The Lavini di Marco is composed of at least two different rock avalanche bodies, the main deposit known as Lavini di Marco (the principal) and the much smaller Costa Stenda deposit. Costa Stenda deposits overlie Lavini di Marco deposits. Samples for ³⁶Cl exposure dating were collected from boulders within the deposits, from sliding plane bedrock and from the bedrock wall at the head scarp. Exposure ages range from 800 ± 210 to 21310 ± 1000 years. The latter age stands as a notable outlier suggesting that that Costa Stenda boulder was exposed for a considerable amount of time in the pre-slide bedrock. Lavini di Marco and Costa Stenda boulder ages are 2600 ± 200, 2700 ± 200, 3100 ± 300, 3300 ± 300, 3400 ± 300, 4400 ± 290, 5300 ± 300, and 5400 ± 300 years. The latter three are Costa Stenda boulders which we also interpret to contain inherited nuclide concentrations. The five remaining boulder ages cluster around 3000 years. We calculate a mean age for the Lavini di Marco and Costa Stenda rockslides of 3000 ± 400 years. Within the uncertainties of our data the two slides were simultaneous. For the bedrock sliding plane we obtained significantly younger ages, 1600 ± 100 and 1400 ± 100 years, and for the head scarp 800 ± 200 years. The sliding plane ages record small-scale reactivation which seems to overlap in time with a catastrophic flood event of the Adige River in Verona, as reported in the Fulda Annales, in 883 AD. Only the single age of 800 ± 210 years suggests activity at Lavini di Marco coincident with the well-known Verona earthquake (1117 AD).     

Timing for high lake levels of Qinghai Lake in the Qinghai-Tibetan Plateau since the Last Interglaciation based on quartz OSL dating

Qinghai Lake is situated in the northeast of the Qinghai-Tibetan Plateau (QTP). Its size and proximity to the junction of three major climate systems make it sensitive to climate changes. Some investigations on shorelines of Qinghai Lake suggested highstands during MIS 3, but to what extent the lake level was higher than today is yet undetermined. Others proposed that the maximum highstands probably dated to MIS 5. It has also been shown that the lake level 120 m higher than today occurred at around 12 ka. Most of these previous ages were obtained using ¹⁴C dating or multiple-aliquot IRSL/OSL dating. For ¹⁴C dating, because of the dating limit (<40 ka) and the lack of suitable dating materials in this arid area, it is difficult to establish reliable chronological control. In the present study, seven samples collected from lacustrine deposits (five samples) and sand wedges (two samples) were dated using quartz optically stimulated luminescence (OSL) with the single aliquot regenerative-dose (SAR) protocol. OSL dating results showed that (1) the lake had experienced two high lake levels, one was in MIS 5 and another in early to middle MIS 3; (2) no evidence of high lake levels in MIS 4 has been found; (3) the alluvial gravels, whose surface is at an elevation of ～3246 m, were formed at least 28.8 ± 2.3 ka ago, and the widespread sand wedges within the alluvial gravels were formed during the period of 15.1–28.8 ka, which implied that the lake level had not reached an elevation of ～3240 m after 28.8 ± 2.3 ka.     

High-precision 40Ar/39Ar dating of pleistocene tuffs and temporal anchoring of the Matuyama-Brunhes boundary

High-precision ⁴⁰Ar/³⁹Ar ages for a series of proximal tuffs from the Toba super-volcano in Indonesia, and the Bishop Tuff and Lava Creek Tuff B in North America have been obtained. Core from Ocean Drilling Project Site 758 in the eastern equatorial Indian Ocean contains discrete tephra layers that we have geochemically correlated to the Young Toba Tuff (73.7 ± 0.3 ka), Middle Toba Tuff (502 ± 0.7 ka) and two eruptions (OTTA and OTTB) related to the Old Toba Tuff (792.4 ± 0.5 and 785.6 ± 0.7 ka, respectively) (⁴⁰Ar/³⁹Ar data reported as full external precision, 1 sigma). Within ODP 758 Termination IX is coincident with OTTB and hence this age tightly constrains the transition from Marine Isotope Stage 19–20 for the Indian Ocean. The core also preserves the location of the Australasian tektites, and the Matuyama-Brunhes boundary with Bayesian age-depth models used to determine the ages of these events, c. 786 and c. 784 ka, respectively. In North America, the Bishop Tuff (766.6 ± 0.4 ka) and Lava Creek Tuff B (627.0 ± 1.5 ka) have quantifiable stratigraphic relationships to the Matuyama-Brunhes boundary. Linear age-depth extrapolation, allowing for uncertainties associated with potential hiatuses in five different terrestrial sections, defines a geomagnetic reversal age of 789 ± 6 ka. Considering our data with respect to the previously published age data for the Matuyama-Brunhes boundary of Sagnotti et al. (2014), we suggest at the level of temporal resolution currently attainable using radioisotopic dating the last reversal of Earths geomagnetic field was isochronous. An overall Matuyama-Brunhes reversal age of 783.4 ± 0.6 ka is calculated, which allowing for inherent uncertainties in the astronomical dating approach, is indistinguishable from the LR04 stack age (780 ± 5 ka) for the geomagnetic boundary. Our high-precision age is 10 ± 2 ka older than the Matuyama-Brunhes boundary age of 773 ± 1 ka, as reported previously by Channell et al. (2010) for Atlantic Ocean records. As ODP 758 features in the LR04 marine stack, the high-precision ⁴⁰Ar/³⁹Ar ages determined here, as well as the Matuyama-Brunhes boundary age, can be used as temporally accurate and precise anchors for the Pleistocene time scale.     

OSL-dating the Quaternary landscape evolution in the Vértes Hills forelands (Hungary)

Fluvial, colluvial, and aeolian sediments were dated by optically stimulated luminescence (OSL) on quartz to improve the chronological framework for Quaternary sedimentation and landscape evolution in the forelands of the Vértes Hills (central Hungary). The separated quartz was suitable for age determination based on an OSL SAR protocol. Most samples have asymmetric equivalent dose distributions and OSL ages were calculated by the mean, central, and minimum D_e values. Considering geomorphology and earlier age data from the area, the central D_e values seem most appropriate for age calculation. A fan on the geomorphological level QV in the western foreland of the Vértes Hills was deposited 79–75 (±8) ka ago. In the south-eastern foreland an alluvial fan on level QIIb is at most 42 ± 4 ka old. Fluvial incision and aggradation occurred 16–10 (±1) ka ago on the geomorphic surface QIIa. Loess is 14 ± 1 ka old, and slope sedimentation was active 11–9 (±1) ka ago. Our OSL data demonstrate that in the north-western foreland of the Vértes Hills wind remained an important agent after the last glacial times, into the early Holocene (9–8 ± 1 ka) and was able to accumulate large aeolian dunes.     

ESR dating of Pleistocene archaeological localities of the Nihewan Basin,North China – Preliminary results

The well-developed, late Cenozoic Nihewan Beds in northern China are amongst the most famous and well-preserved Quaternary strata in East Asia. The Nihewan Basin is also well-known for its mammalian fossils and stone artifacts, which document early human settlements in high northern latitudes (around 40°N). It is a key geological place to study palaeoenvironments and ancient human activities due to the excellent age-control of the formation by palaeomagnetism. In the present paper, the sediments of two Paleolithic sites were dated using the ESR signals of the titanium center in quartz. In order to check the reliability of our analytical procedures, a reference sample collected near the Brunhes/Matuyama (B/M) boundary at the Donggutuo site was firstly analyzed, yielding an age of 750 ± 88 ka. Then, three samples collected from the Dongpo site were analyzed by the same procedures. Our ESR results indicate that the age of the Dongpo cultural layer ranges between 304 ± 12 ka and 333 ± 23 ka, with an average of approximately 321 ± 15 ka.     

When were the walls of the Chauvet-Pont d'Arc Cave heated? A chronological approach by thermoluminescence

Direct chronological data of the ancient heating of calcitic walls at the Chauvet-Pont d'Arc Cave (Ardèche, France) were obtained at the Galerie des Mégacéros and at the Eboulis d'Entrée. Fragments of reddened limestone were extracted from the walls and were studied by thermoluminescence (TL). A novel measurement protocol of the equivalent dose (ED) was implemented and was optimized with respect to the nature of the material being dated (calcite), to the small quantities of sample available and to the relatively low heating of the rock surface in the past (close to 350 °C). The presence of a high level of free radon in the cave and ²¹⁰Pb in large excess in samples implied the development of a specific irradiation model allowing the evaluation of the mean annual dose over time, taking into account possible scenarios of radon and daughters migration from the bedrock. The following dating results were obtained (in ka before the present and associated total estimated standard deviation):- Galerie des Mégacéros, 36.9 ± 2.3 ka.- Eboulis d'Entrée, 34.3 ± 2.9 ka.These data are in agreement with the calibrated radiocarbon dates of the most ancient periods of human occupation in their respective areas. TL dates indicate that the fires which altered the walls were lighted during the first paleolithic human occupation period. Eventually, TL dating of the heated surface of the bedrock opens a new window on the chronology of human activities in the Chauvet-Pont d'Arc Cave and it makes an alternative contribution to the demonstration of the early chronology of its rock art.     

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 dating of quartz phenocrysts in the El Cajete and Battleship Rock Members of Valles Rhyolite, Valles Caldera, New Mexico

The electron spin resonance (ESR) dating method was employed on quartz phenocrysts separated from pumice of the El Cajete and Battleship Rock Members of the Valles Rhyolite in the Valles caldera, New Mexico. The results of heating experiments indicate that Ti impurity centers have two components; a thermally stable one and a less stable, temperature sensitive one. ESR dates using the stable Ti center yield eruption ages of 59 ± 6 ka for the Battleship Rock Member and 53 ± 6 ka for the El Cajete Member while recent ¹⁴C dates (S. Reneau and J. Gardner, unpub. data) from carbonized logs in the El Cajete pumice indicate that its age is older than 50 ka. Our results indicate that volcanism in the Valles caldera is much younger than previously thought (≥ 130 ka) and that recent revisions to the post-0.5 Ma stratigraphy of Valles caldera are probably in error. The results suggest that ESR dating of quartz may be a useful method for obtaining ages of units in other Quaternary volcanic areas.