Isochron 26Al/10Be burial dating of the Lantian hominin site at Gongwangling in Northwestern China

The site of Gongwangling is among the most important early hominin sites in China due to the discovery of a partial Homo erectus cranium. Until recently the cranium has been widely accepted as ∼1.15 Ma (million years) in age based on magnetostratigraphy and loess/paleosol correlation. However, a revised magnetostratigraphic and pedostratigraphic study assigned a much older age of 1.63 Ma, making Gongwangling the second oldest hominin cranium-bearing site in Eurasia. Here we apply the isochron burial dating method as an independent check for the magnetostratigraphy. Samples from the top of a gravel bed ∼7 m below the fossil-bearing layer give an isochron burial age of 1.82 ± 0.12 Ma, in excellent agreement with the Olduvai subchron in the revised magnetostratigraphy, supporting the antiquity of the cranium.     

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

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

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).     

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

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

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.     

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.     

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

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

230Th/U chronology of a paleolithic site at Xinglong Cave in the three-Gorge region of south China

Xinglong Cave, containing four human teeth, numerous mammalian fossils, stone artifacts and a Stegodon tusk with intentional and seemingly grouped engravings, is one of the most significant archaic Homo sapiens sites in south China, located 95 km south of Fengjie County, in Chongqing. In an attempt to constrain the age of the human relics, calcitic flowstone deposits with a significant detrital component were dated by U–Th methods using a leachate scheme. Total sample digestion MC-ICPMS dating was used to assess the reliability of the leachate technique. Six calcite samples from horizons beneath and above the fossil-bearing layer were dated. We obtained ages of 130 ± 9.1, 124 ± 11, 135 ± 12 and 127 ± 11 ka for the flowstones above the fossil layer with a weighted mean of 128.9 ± 5.2 ka. Two flowstone samples gave MC-ICPMS dates between 128.3 ± 3.3 and 152.4 ± 25.3 ka with an assumed detrital component to correct for the initial ²³⁰Th, which are consistent with results obtained using the L/L regression data from layer U-4 within uncertainty. All errors herein quoted at the 2σ level. Ages determined for the flowstone underlying the fossil-bearing layer were 221 ± 29 to 189 ± 19 ka with a weighted mean age of 199 ± 16 ka. These results are stratigraphically consistent within error limits and show that the cave was occupied by Fengjie Man within the time range of ∼200 to ∼130 ka. These new U-series ages of flowstones in association with human teeth and an engraved stegodon tusk at the Xinglong Cave site provide valuable geochronologic information for the study of the origin of modern humans in East Asia and earliest human art.     

A targeted drilling and dating campaign to identify Stone Age archaeological sites before excavation in west coast southern Africa

Here we present the results of a targeted drilling campaign that facilitated a geochronological study with coarse sampling resolution inside a new cave site, Simons Cave, on the west coast of southern Africa. A combination of radiocarbon (¹⁴C) dating and optically stimulated luminescence (OSL) dating was used as a range-finder. Results confirmed preservation of Holocene and late Pleistocene sediments up to 133 ± 35 ka, overlapping with the ages of Middle Stone Age (MSA) occupations of the broader west coast region. A subsequent, systematic test-excavation at the site then embarked on a second geochronological study with a higher sampling resolution. Ultimately, the comparative study confirmed the potential of Simons Cave as a new site for the exploration of hominin occupation through the later Pleistocene and Holocene, yet raised several issues concerning the direct comparability of information deriving from drilled sediment cores and actual archaeological excavation.     

Cosmogenic isotope burial dating of fluvial sediments from the Lower Rhine Embayment,Germany

Cosmogenic isotope burial dating, using ¹⁰Be and ²⁶Al, was applied to Plio–Pleistocene fluvial successions from the Lower Rhine Embayment, Germany. The approach consists of three principal steps: (1) measurement of cosmogenic nuclides in depth profiles, (2) modelling of hypothetical nuclide concentrations based on a first-order conceptualisation of the geological context and the principal succession of depositions and subsequent erosional and burial phases, and (3) using parameter estimation to identify values for the a priori unknown model parameters (burial age, initial nuclide concentrations, terrace erosion rates) that result in minimal disagreement between hypothetical and measured nuclide concentrations.The Late Pliocene Kieseloolite Formation was dated to 3650 ± 1490 ka and the Early Pleistocene Waalre Formation to 900 ± 280 ka. The unconformably overlying Upper Terrace Formation revealed ages of 740 ± 210 ka and 750 ± 250 ka for the two different sites. These findings are in good agreement with independent age control derived by bio-, magneto-, and litho-stratigraphy. Furthermore, identifiability and uncertainty analysis reveal a relationship between burial depth and sensitivity of isotope concentrations to burial age and erosion rate. Our results indicate that using shallower buried samples would enable a considerably more robust estimation of the burial age and the terrace erosion rate. Uncertainties arose mainly from nuclide measurements, and not from the uncertainties derived from modelling or insufficient knowledge of nuclide production and decay properties.     

Evaluating Quaternary dating methods: Radiocarbon,U-series,luminescence, and amino acid racemization dates of a late Pleistocene emu egg

A whole emu egg, with infilling sediment believed to be coeval with egg laying and burial, was found in late Pleistocene lunette sediments near Lake Eyre, central Australia. The stratigraphic context and initial amino acid racemization (AAR) results suggested an age between 25 ka and 35 ka, ideal for a multiple cross-dating comparison. The sediment infilling the egg provided material for luminescence dating that minimized problems of association. Age estimations from AAR, ¹⁴C and U series methods were obtained from the eggshell and optically stimulated luminescence (OSL) of the infilling sediment. All methods agreed within their respective dating uncertainties confirming the utility of all four methods. They indicate an age for the emu egg of 31.24 ± 0.34 ka.     

Chronology analysis of huge landslide based on ESR dating materials on sliding face in carbonate areas of south eastern Tibet

Determining occurrence age is key to chronology analysis of huge landslides. However, in carbonated bedrock areas, it is difficult to carry out geochronological surveys of landslide evolution due to lack of suitable dating materials and methods. In carbonated bedrock areas, the cosmic nuclides 36Cl and 14C dating methods have been used for obtaining the exposed age of bedrock. But intense weathering, erosion and dissolution make it difficult to obtain an accurate total amount of cosmogenic nuclide accumulation, resulting in the dating results being affected greatly by weathering, erosion and dissolution of carbonate rock. Therefore, it is necessary to find new dating materials or methods for determining the occurrence age of landslide in carbonate bedrock areas with little quaternary sediments. In this study, a huge landslide developed in the carbonate bedrock area of south eastern Tibet is introduced briefly, which is named the Qiaojia landslide and blocked the Jinsha River. A thin layer including three obvious recrystallized carbonate sub-layers was formed in the sliding zone, indicating different sliding events. Three recrystallized carbonate samples were then collected for ESR dating research to obtain the age information of the Qiaojia landslide: one occurred 79 ± 8 ka years ago, and the other occurred 60 ± 10 ka years ago, and the third occurred 25 ± 2 ka years ago, which are in general agreement with other studies in the surrounding of the study area. It suggests that recrystallized carbonate on sliding face is suitable for chronologically identifying landslide activity by using ESR method in the carbonate area, especially in the areas with little or no quaternary sediments.     

MET-post-IR IRSL luminescence dating of cobbles buried in fluvial terraces in the Northern Chinese Tian Shan

Cobbles can be used as an alternative to the conventionally employed sand-sized mineral luminescence dating. In piedmont environments, cobbles are much more abundant than sand-sized material. The IRSL₅₀ signal has been widely used in previous studies due to its greater sensitivity to exposure events. However, it is well known that the low temperature IRSL signal is more prone to fade than elevated temperature post-IR IRSL signal. In this study, to test the reliability and applicability of cobble sub-surface elevated temperature IRSL luminescence dating, six light-color granite cobbles and two sand-sized samples from silty sand lens were collected from a high terrace of Manas River on the northern piedmont of Chinese Tian Shan. A modified multi-elevated-temperature post-infrared infrared stimulated luminescence (MET-post-IR IRSL) protocol was applied. The age-temperature (A-T) plateau of MET-post-IR IRSL measurement was combined with the conventional age-depth (A-D) plateau in luminescence-depth profile to evaluate the resetting and fading of MET-post-IR IRSL signals. Uncertainties of grain-sizes of K-feldspar within solidified slices were also explored by μ-XRF mapping of potassium content. The A-T plateau was identified between MET-post-IR IRSL₁₇₀ and MET-post-IR IRSL₂₂₅ signals of one cobble, which suggested completeness of bleaching before burial and negligible anomalous fading during burial. This cobble yielded MET-post-IR IRSL₂₂₅ ages of 15.8 ± 2.6 ka and 19.0 ± 3.2 ka for top and bottom side, respectively. These MET-post-IR IRSL₂₂₅ ages were consistent with independent coarse-grained quartz MAM OSL ages (15.7 ± 3.6 ka and 14.8 ± 2.6 ka) of two sand-sized samples. The MET-post-IR IRSL₂₂₅ age of 16.0 ± 1.2 ka for the bottom side of another cobble was also consistent with the independent age, even without the A-T plateau. It was inferred to be caused by anomalous fading of MET-post-IR IRSL signals other than that stimulated at 225 °C by refering to the A-D plateau observed. Our results show that MET-post-IR IRSL measurement can be employed to determine the burial ages of cobbles. The A-T plateau, complemented with the A-D plateau, could be used to assess the reliability of burial ages of cobble luminescence dating from the view of bleaching and fading.     

Luminescence dating of baked earth and sediments from the Qujialing archaeological site,China

The Qujialing site is a representative Neolithic archaeological site in the middle reaches of the Yangtze River, China. Absence of suitable material for radiocarbon dating in this region makes the timing of the similar sites difficult. Here we applied optically stimulated luminescence (OSL–SAR) and thermoluminescence (TL–SAR) techniques to date the archaeological and natural deposits from the Qujialing site with known age, testing the techniques on samples at archaeological sites in this region. The results showed that the luminescence properties of quartz from sediment and baked earth samples are very similar. The quartz OSL ages obtained for a sediment sample and a baked earth sample from the cultural layer are 5.4 ± 0.3 and 5.1 ± 0.3 ka, respectively. The quartz TL age of the baked earth sample is 5.6 ± 0.5 ka. These dates are consistent with the calibrated radiocarbon ages (4.9 ± 0.1 and 5.1 ± 0.1 ka cal BP (±1σ)) of the two charcoal samples from the cultural layer at a nearby locality, and are also in agreement with the age of Qujialing culture period. The results indicate that the OSL dating techniques can be applied to date similar archaeological sites in the middle reaches of the Yangtze River, China.     

Luminescence dating of sediments from a Palaeolithic site associated with a solution feature on the North Downs of Kent,UK

Optically stimulated luminescence (OSL) dating has been applied to determine the burial age of sediment horizons within a sequence containing Lower Palaeolithic artefacts on an upland site associated with a solution feature (doline) at West Cliffe, located on the North Downs in Kent, UK. The study makes use of a novel extension of the single aliquot OSL measurement procedure to investigate the nature of significant overdispersion in equivalent dose values with very small aliquots of quartz inclusions, enabling single grain resolution to be approached with ∼90 μm diameter quartz extracted from the relatively fine-grained brickearth. A detailed examination of the uniformity of the distribution of radionuclide sources in the sampled volumes was also performed and this included the application of a spatially-resolved technique for beta dose rate measurement. The OSL ages, obtained for the burial of brickearth positioned stratigraphically below and above a clay and flint clast layer containing the artefacts and debitage, place the deposition of the artefacts to between ca 140 and 80 ka ago. This is significantly later than indicated by the artefact typology (>300 ka) and contrary to the expectation of in situ burial indicated by earlier research in this region. If displacement occurred on other upland sites this finding has important implications for establishing the timing of hominin use of the upland areas which, beyond broad attribution to Lower or Middle Palaeolithic origin, is uncertain and similar doubts apply to the interpretation of the environments that prevailed.     

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

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

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.     

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.     

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.     

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

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