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

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

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

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

New chronological constraints for the lowermost stratigraphic unit of Atapuerca Gran Dolina (Burgos,N Spain)

We present the results of a combined Electron Spin Resonance (ESR) and Luminescence dating study for the lowermost stratigraphic unit (TD1) of the palaeoanthropological site of Atapuerca Gran Dolina, Spain. Ten samples collected through the Main Section were dated using either the Multiple Centre (MC) ESR approach or the single-grain thermally transferred optically stimulated luminescence (SG TT-OSL) technique, both of which were applied to quartz grains. The two methods yield consistent ages, providing a robust chronostratigraphic framework for the TD1 deposits and enabling improved correlation of the magnetostratigraphic succession (comprising three intervals of normal polarity; N1 to N3, from bottom to top) with the Geomagnetic Polarity Time Scale. Specifically, the results provide a late Early Pleistocene chronology for TD1, and clearly position the deposits in the post-Olduvai time range (<1.77 Ma). The final age estimates range from 1.30 ± 0.14 Ma (TT-OSL) close to the bottom of the section to a mean ESR age of 1.05 ± 0.12 Ma (1 s.d.) for three samples from the N3 interval towards the top. Consequently, the N3 interval may confidently be correlated to the Jaramillo Subchron, while we propose a correlation of N1 and N2 with the Cobb Mountain subchron and Punaruu excursion, respectively; although we cannot exclude that these two normal intervals may correspond to other, unknown, geomagnetic events given the existing uncertainties associated with the ESR and luminescence ages.From a methodological point of view, the ESR MC approach shows that the Titanium signal provides the most reliable burial ages for TD1. In contrast, the Aluminium centre yields systematically overestimated age estimates, as a result of incomplete resetting of the signal before sediment deposition. The SG TT-OSL ages presented here are amongst the oldest published so far, and highlight the potential of the high temperature SG TT-OSL₂₉₀ approach for obtaining finite ages exceeding 1 Ma at Atapuerca.Finally, these new dating results provide key insights into the rates and nature of sedimentary processes at Gran Dolina, modifying long-standing interpretations of the cave formation and infilling dynamics. An age of at least 1.4 Ma may be inferred for the base of the sedimentary infill at the Main Section, providing minimum age constraint for the formation of the cavity and, by extension, for the intermediate level of the Atapuerca karst. The opening of the cave, which pre-dates human occupation, most likely occurred close to or slightly after 0.9 Ma. This suggests that both TD4 and TD6 archaeological levels were deposited within a relatively short time range of <100 kyr. The so-called autochthonous fluvial deposits from TD1 unit, or at least those dated in the present study, were also clearly primarily derived from outside the karst system, and were not reworked from older deposits within the karst. They experienced sufficient daylight exposure and minimum transport times within the karst system to enable consistency between the ESR and TT-OSL burial ages and the independent magnetostratigraphic evidence. Our results highlight the need to reconsider the terminology traditionally employed to differentiate the two main phases of Gran Dolina's sedimentary infill.     

OSL dating of individual quartz ‘supergrains’ from the Ancient Middle Palaeolithic site of Cuesta de la Bajada,Spain

Dose saturation represents a fundamental limitation for obtaining finite optically stimulated luminescence (OSL) quartz ages over Middle Pleistocene timescales. Single-grain OSL studies typically reveal significant intra- and inter-sample variability in quartz dose saturation properties at the individual grain level. This enhanced variability may offer the potential to obtain extended-range chronologies exceeding the traditional upper age limits of multiple-grain OSL dating. However, there have been relatively few detailed assessments of single-grain OSL properties over high dose ranges. In this study we investigate extended-range single-grain OSL dating potential at Cuesta de la Bajada, one of the most important Ancient Middle Palaeolithic sites in the Iberian Peninsula. The quartz samples from this site exhibit exceptional dose saturation properties and contain significant populations of individual ‘supergrains’ with bright OSL signals, very high characteristic saturation dose (D₀) limits of 200 to >600 Gy, and dose-response curves that closely conform to single saturating exponential functions. Assessments of OSL signal composition and the ability to successfully recover a known laboratory dose of 470 Gy support the potential for obtaining high equivalent dose (D_e) values with reasonable fitting uncertainties. A series of novel sensitivity tests are used to assess potential biases in supergrain D_e estimation over high dose ranges related to (i) thermally transferred signal contributions, (ii) choice of dose-response curve fitting function, and (iii) insufficient dose saturation properties of individual grains. The single-grain D_e values obtained using the standard quality assurance criteria and novel sensitivity tests are consistent at 2σ, and are in agreement with quartz Ti-centre ages obtained on two of three paired electron spin resonance (ESR) samples collected from Cuesta de la Bajada. These comparisons support the suitability of our single-grain OSL results and suggest there may be good potential for using quartz supergrains to establish extended-range chronologies at some Middle Pleistocene sites. Comparisons with other single-grain OSL studies across the Iberian central plains suggest that favourable dose saturation properties may be influenced by regional-scale geological controls. The importance of undertaking single-grain OSL dating at Cuesta de la Bajada is also demonstrated by the results of synthetic aliquot experiments, which reveal multiple-grain age offsets of 60–170 ka when unsuitable grain types are inadvertently included in the final age calculations. The single-grain OSL results indicate that the main archaeological horizon at Cuesta de la Bajada (unit CB3) accumulated between 264 ± 22 and 293 ± 24 ka. These ages are consistent with the chronologies of other key early Middle Palaeolithic sites in the region (Ambrona AS6 and Gran Dolina TD10) and indicate that the Ancient Middle Palaeolithic techno-complex likely spread across Iberia from at least Marine Isotope Stage 9 onwards.     

Re-evaluation of the chronology of the palaeolithic site at Jeongokri,Korea, using OSL and TT-OSL signals from quartz

Seven samples were collected from sediments at the Palaeolithic site of Jeongokri, Korea, known for the first discovery of Acheulian-like handaxes in East Asia. Optically stimulated luminescence (OSL) ages obtained from chemically purified quartz from the upper five samples are in stratigraphic order, but the ages of the lower samples are not. The OSL signal of the oldest samples occurs well above the saturation level of the exponential part of the dose response curve; however, the OSL signal has an additional component that grows linearly at high doses, making it possible to calculate a D_e value and thus an age. However the reliability of calculating D_e using this linear component is not clear. In contrast, the thermally transferred OSL (TT-OSL) signal grows linearly with dose up to at least 1600 Gy, thus permitting its use for dating. The TT-OSL ages are in agreement with those from the OSL for the four uppermost samples, but give older ages for the lower three samples. Ages obtained using TT-OSL are in stratigraphic order and indicate that the oldest artefacts have an age of ～195 ka.     

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.     

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.     

Exploring fading in single grain feldspar IRSL measurements

IR laser stimulated luminescence was used to determine the equivalent dose (D_e) for about 150 luminescent K-feldspar grains of two well-bleached aeolian sand samples, previously dated using quartz optically stimulated luminescence (OSL) and thermally-transferred OSL (TT-OSL). Fading tests were performed both on the entire single grain disc, using stimulation by IR LEDs, and on each grain individually, by stimulation with an IR laser. The single grain D_e distributions are highly over dispersed, even after applying rejection criteria, such as recycling ratio and recuperation. Fading rates determined with the IR LED stimulation do not represent the fading behavior of the IR laser stimulated signal and are therefore considered inappropriate for the fading correction of single grain D_e values. Fading rates of individual grains exhibit a wide range of values (0%–10% per decade) and plotting the single grain fading rates against the single grain D_e values reveals a negative relationship. Different approaches were taken to correct for fading, but the resulting ages tend to underestimate the reference ages.     

Optical dating of perennially frozen deposits associated with preserved ancient plant and animal DNA in north-central Siberia

We present chronological constraints on a suite of permanently frozen fluvial deposits which contain ancient DNA (aDNA) from the Taimyr Peninsula of north-central Siberia. The luminescence phenomenology of these samples is first discussed, focusing on the optically stimulated luminescence (OSL) decay curve characteristics, thermoluminescence (TL) properties, and signal compositions of quartz from these previously unstudied deposits. Secondly, we assess the suitability of these samples for OSL dating and present the OSL chronologies obtained using both single-grain and multi-grain equivalent dose (D_e) measurements. The results of our analyses reveal a large amount of inter-aliquot variability in OSL decay curve shape that is directly related to differences in the size of the 280 °C TL peak and the associated slowly bleached ‘S2’ OSL component. Longer OSL stimulation durations are adopted in the D_e measurement procedure to prevent the progressive build-up of slowly bleached signal components throughout successive single-aliquot regenerative-dose (SAR) measurement cycles. The use of low preheat temperatures in the SAR procedure also reduces the deleterious effects of these slowly bleached signal components. The resultant single-grain and multi-grain OSL chronologies obtained using this approach are stratigraphically consistent and are in close agreement with independently established ¹⁴C ages at our sites. The findings of this research reveal the potential of OSL dating as a means of providing a reliable chronometric framework for sedimentary aDNA records in permafrost environments.     

Evaluating a SAR TT-OSL protocol for dating fine-grained quartz within Late Pleistocene loess deposits in the Missouri and Mississippi river valleys,United States

The Mississippi and Missouri river valleys in the midcontinental United States contain extensive loess-paleosol sequences that are used to constrain the timing of expansion and retreat of the Laurentide Ice Sheet. Previous studies have been unsuccessful in producing finite ages for sediments older than ∼150 ka due to saturation of luminescence emissions. The thermally transferred optically stimulated luminescence (TT-OSL) dating technique is tested on the fine-grained (4–11 μm) quartz fraction of these loess deposits because the TT-OSL signal has been shown to grow with high (kGy) radiation doses. The TT-OSL signal continued to increase with radiation dose above 900 Gy. The optical and thermal stabilities of this TT-OSL signal are evaluated. Equivalent dose values are highly sensitive to preheat temperatures. Recycling ratios, zero-dose response values, and dose recovery tests all yield acceptable values for samples with burial doses >∼200 Gy. The apparent TT-OSL ages for the Roxana Silt (∼52–63 ka), Teneriffe Silt (∼66 ka), and Loveland Silt (∼133–192 ka) agree at 1σ level with previously published TL and IRSL ages derived from the same samples. For the oldest unit, the Crowley's Ridge Silt, TT-OSL ages (∼167–200 ka) are younger than IRSL or TL ages by ∼20%. This is interpreted as underestimation related to TT-OSL signal contamination, which can be avoided by isolating the fast component of the TT-OSL. Preliminary fast component TT-OSL ages for the Crowley's Ridge Silt (∼197–241 ka) favor deposition during marine oxygen-isotope stage (MIS) 7 or 8, contrary to a previous inference of a MIS 12 deposition.     

Residual OSL signals in modern fluvial sediments from the Yellow River (HuangHe) and the implications for dating young sediments

The Yellow River is characterized by its tremendous sediment load. In this study we investigated the residual OSL signals in modern fluvial sand and suspended-sediment samples from the middle reach of the river. The residual equivalent dose (D_e) is found to vary with grain size, mineralogy and the techniques used for the D_e determination. The results indicate that the OSL signals in some grains from these samples were not completely bleached prior to burial, the maximum individual D_e value obtained is up to 56 Gy. The results also show that coarse grains are generally better bleached at deposition than fine grains; the fine-grained quartz from suspended sediments are better bleached than the fine-grained quartz from the fluvial sand deposits. The D_es obtained using quartz TT-OSL signals are up to ～380 Gy for these modern samples.     

The effect of single grain luminescence characteristics on single aliquot equivalent dose estimates

We report an investigation of the effect of different single grain OSL behaviours on multiple-grain (single aliquot) D_e estimates. This was done by creating ‘synthetic aliquots’ in which signals are summed from collections of individual grains. The samples used were taken from aeolian linear dune sediments, from sites located in the Kalahari. We note this is a type of sample for which single multiple-grain aliquots are routinely used for dating. Several grain behavioural types were identified in our samples but the only grain type that systematically affected multiple-grain D_e estimates was the ‘over-saturating’ type (the case where the natural signal (L_n/T_n) is significantly greater than the regenerated L_x/T_x signal at saturation), the presence of which lead to higher estimates of D_e. The magnitude of this effect is controlled by the contribution of ‘over-saturating’ grains to the total light sum of the multiple-grain aliquot and the maximum increase observed in this study was ∼15 Gy. Of the four samples investigated here, inter-aliquot variations in the signal contribution of ‘over-saturating’ grains led to a significant increase in dispersion in just one of the samples. More generally, the presence/absence of these grains is considered to be a likely source of significant ‘intrinsic’ scatter in single aliquot dating and likely to broaden multiple-grain D_e distributions. We suggest all samples are screened for this behaviour before single aliquot dating is attempted.     

A revised burial dose estimation procedure for optical dating of youngand modern-age sediments

The presence of genuinely zero-age or near-zero-age grains in modern-age and very young samples poses a problem for many existing burial dose estimation procedures used in optical (optically stimulated luminescence, OSL) dating. This difficulty currently necessitates consideration of relatively simplistic and statistically inferior age models. In this study, we investigate the potential for using modified versions of the statistical age models of Galbraith et al. [Galbraith, R.F., Roberts, R.G., Laslett, G.M., Yoshida, H., Olley, J.M., 1999. Optical dating of single and multiple grains of quartz from Jinmium rock shelter, northern Australia: Part I, experimental design and statistical models. Archaeometry 41, 339–364.] to provide reliable equivalent dose (D_e) estimates for young and modern-age samples that display negative, zero or near-zero D_e estimates. For this purpose, we have revised the original versions of the central and minimum age models, which are based on log-transformed D_e values, so that they can be applied to un-logged D_e estimates and their associated absolute standard errors. The suitability of these ‘un-logged’ age models is tested using a series of known-age fluvial samples deposited within two arroyo systems from the American Southwest. The un-logged age models provide accurate burial doses and final OSL ages for roughly three-quarters of the total number of samples considered in this study. Sensitivity tests reveal that the un-logged versions of the central and minimum age models are capable of producing accurate burial dose estimates for modern-age and very young (<350 yr) fluvial samples that contain (i) more than 20% of well-bleached grains in their D_e distributions, or (ii) smaller sub-populations of well-bleached grains for which the D_e values are known with high precision. Our results indicate that the original (log-transformed) versions of the central and minimum age models are still preferable for most routine dating applications, since these age models are better suited to the statistical properties of typical single-grain and multi-grain single-aliquot D_e datasets. However, the unique error properties of modern-age samples, combined with the problems of calculating natural logarithms of negative or zero-Gy D_e values, mean that the un-logged versions of the central and minimum age models currently offer the most suitable means of deriving accurate burial dose estimates for very young and modern-age samples.     

Equivalent dose estimation of calcite using isothermal thermoluminescence signals

Thermoluminescence (TL) signals of calcite can be used to potentially date geological and archaeological events back to several million years. However, several issues, such as spurious TL signals appearing at temperatures above 300 °C, have hindered its application to a wide range of samples. A single-aliquot regenerative-dose (SAR) protocol for calcite with low-temperature measurements is proposed to measure the equivalent dose (D_e). It uses the isothermal TL (ITL) signals measured at around 225-240 °C, where a D_e vs. ITL temperature (D_e-T) plateau can be observed. The width of the temperature range of such a plateau can be sample dependent, as it relates to the proportional contributions of the signals from corresponding TL peaks. The signal at the ITL temperature plateau range largely corresponds to the TL signals of the 280 °C TL peak. D_e values obtained by the SAR-ITL protocol are in agreement with those of the multiple-aliquot additive-dose (MAA)-TL and MAA-ITL protocols. The absence of detectable anomalous fading of ITL signals at 235 °C in this and previous studies indicates that the signal is free of fading. Dose recovery tests confirm the suitability of the SAR-ITL protocol for D_e estimation. The SAR-ITL protocol measured with temperatures below 300 °C avoids the effects of spurious luminescence signals induced by high-temperature heating. The dose-response curves for ITL signals at 230-235 °C have large characteristic saturation doses (D₀) of ∼2000-2400 Gy. The SAR-ITL protocol for calcite thus has the potential to date geological and archaeological samples spanning the entire Quaternary period.     

Examining sediment infill dynamics at Naracoorte cave megafauna sites using multiple luminescence dating signals

Relatively little is known about the long-term sediment accumulation dynamics of Naracoorte Cave Complex (NCC) solution pipe cavities, and many of the megafauna-bearing infill deposits at this globally significant Australian Pleistocene fossil locality remain partially dated or lack any numerical age control. In this study, we assess the suitability of three different luminescence dating signals for improving existing chronologies at six Late and Middle Pleistocene NCC sites (n = 22 samples), and we undertake multi-site examinations of NCC sediment infill dynamics spanning the last 550 thousand years (ka). Modern analogue samples collected from above and beneath two active cave entrances confirm that single-grain OSL, single-grain TT-OSL and multi-grain pIR-IRSL signals can be reset down to insignificant residual levels (<10⁻¹–10⁰ Gy) when compared with the natural dose ranges of interest for most NCC palaeontological applications. Replicate luminescence dating comparisons performed at six NCC fossil sites (n = 15 samples) reveal consistent ages for twenty-eight out of thirty-one paired OSL–TT-OSL, OSL–pIR-IRSL and TT-OSL–pIR-IRSL datasets. Nineteen of the twenty Middle to Late Pleistocene samples analysed from the NCC sites produce homogeneous OSL, TT-OSL and pIR-IRSL D_e datasets suggesting that the NCC solution pipe deposits considered here are generally not affected by syn-depositional mixing complications that can take place within closed karst cavities (i.e., the remobilisation of unbleached grains from pre-existing cave floor sediments, and their subsequent translocation and incorporation into deposits within deeper parts of the cavity along with externally bleached, allochthonous grain populations). Detailed examination of solution pipe dynamics at Smoke Tortoise Cave (SMT) reveals a complex accumulation history focused on the marine isotope stage (MIS) 9 and MIS 7 interglacial complexes, as well as the MIS 8e interstadial. The SMT case study highlights that NCC solution pipes are not simply associated with short-lived opening and sediment accumulation events, but may involve multiple, discontinuous deposition episodes and reactivation events. An initial multi-site examination of all published NCC infill chronologies (n = 70) appears to suggest statistically significant, preferential solution pipe development during the relatively wet parts of interglacial or interstadial cycles. The non-uniform infill age distribution implies that NCC solution pipe dynamics may have exerted taphonomic biases on fossil accumulation, which should be taken into consideration when reconstructing long-term palaeoecological histories from NCC solution pipe cavities.     

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

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

Luminescence dating of volcanic eruptions in Datong,northern China

In this study, fine-grain quartz was used for luminescence dating for lava baked samples from different sites in Datong. Optical stimulated luminescence (OSL), thermal transferred OSL (TT-OSL)/recuperated OSL (Re-OSL) and thermoluminescence (TL) dating protocols were applied. For these samples, the OSL signals saturate at about 300–400 Gy, which limits their age to less than 100 ka based on their ambient dose rates. The TT-OSL/Re-OSL method has poor dose recovery. TL dating gives reliable results, and multiple-aliquot regenerative-dose TL method with sensitivity change correction based on the 325 °C TL peak of a test dose can be applied for samples up to 400 ka. The results indicate that the ages of the volcanoes in Datong are from 380 ka to 84 ka. The volcanic activity started earlier in the southeast area than those in the northwest part, which is consist with the literature data.     

Challenges of dating quartz OSL samples with saturated grains: Lessons from single-grain analyses of low dose-rate samples from Victoria Falls,Zambia

A suite of samples from an extensive aeolian sandscarp near Victoria Falls, Zambia was used to explore several different methods of calculating optically stimulated luminescence (OSL) ages that account for the effects of saturated quartz grains. Beta dose rate heterogeneity and early OSL signal saturation of the samples exacerbate the impact that saturated grains have on the equivalent dose (D_e) values calculated. Saturated grains that cannot calculate D_e values are often rejected but the minimum burial dose information they contain can have a significant impact on a sample's average D_e value. This study compares multiple techniques for combining luminescence measurements that enables inclusion of this data and their sensitivity to a criterion that rejects grains with early OSL signal saturation. The methods tested are found to have different advantages and disadvantages, but reasonable agreement between the D_e values they calculate suggests that including data from saturated grains makes a more significant difference to D_e values calculated than the specific method used to combine the data.     

Small aliquot and single grain IRSL and post-IR IRSL dating of fluvial and alluvial sediments from the Pativilca valley,Peru

Infrared stimulated luminescence (IRSL) and post-IR IRSL are applied to small aliquots and single grains to determine the equivalent dose (D_e) of eleven alluvial and fluvial sediment samples collected in the Pativilca valley, Central Peru at ca. 10°S latitude. Small aliquot D_e distributions are rather symmetric and display over-dispersion values between 15 and 46%. Small aliquot g-values range between 4 and 8% per decade for the IRSL and 1 and 2% per decade for the post-IR IRSL signal. The single grain D_e distributions are highly over-dispersed with some of them skewed to higher doses, implying partial bleaching; this is especially true for the post-IR IRSL. Measurements of a modern analog reveal that residuals due to partial bleaching are present in both the IRSL as well as the post-IR IRSL signal. The g-values of individual grains exhibit a wide range with high individual uncertainties and might contribute significantly to the spread of the single grain D_e values, at least for the IRSL data. Electron Microprobe Analysis performed on single grains reveal that a varying K-content can be excluded as the origin of over-dispersion. Final ages for the different approaches are calculated using the Central Age Model and the Minimum Age Model (MAM). The samples are grouped into well-beached, potentially well-bleached and partially bleached according to the evaluation of the single grain distributions and the agreement of age estimates between methods. The application of the MAM to the single grain data resulted in consistent age estimates for both the fading corrected IRSL and the post-IR IRSL ages, and suggests that both approaches are suitable for dating these samples.     

Bleachability of pIRIR signal from single-grain K-feldspar

The high-temperature (e.g., >200 °C) post-infrared infrared (pIRIR) stimulated luminescence of feldspar has been widely used for dating, because it usually suffers negligibly from anomalous fading. However, compared to the quartz optically stimulated luminescence (OSL) or low-temperature (e.g., 50 °C) IR stimulated luminescence (IRSL) from feldspars, the high-temperature pIRIR signals have been shown to bleach more slowly and usually have high residual does of a few Gys or more, which limits its application to date relatively young samples and may cause problems for correcting residual dose/signal. In this study, we investigated the bleachability of K-feldspar pIRIR signals for individual grains. A significant variation in the bleachability of the pIRIR signal was observed among different K-feldspar grains from the same sample. Experiments show that such a variability may result in different residual doses for different grains and, consequently, additional scatter in D_e values. We present a method for quickly testing the bleachability of individual grains. Our result suggests that selecting the easy-to-bleach grains for D_e determination provides an efficient way to date young samples using high-temperature pIRIR signals, which avoids the compromise of using low-temperature pIRIR signals that may suffer from anomalous fading.