Investigation of the applicability of standardised growth curves for OSL dating of quartz from Haua Fteah cave,Libya

The establishment of standardised growth curve (SGC) for equivalent dose (D_e) determination can substantially reduce the amount of instrument time required for OSL measurements. In this study, we investigated the applicability of SGC for the optically stimulated luminescence (OSL) signal from single grains and small aliquots of sedimentary quartz from Haua Fteah cave, in Libya. The samples exhibit large inter-grain and inter-aliquot variation in the shape of their single grain and small aliquot dose response curves (DRCs) constructed from a range of sensitivity-corrected regenerative dose signals (L_x/T_x), which prevents the establishment of a single common SGC among different grains or small aliquots. Instead, the DRCs for the small aliquots can be divided into a minimum of three groups using the Finite Mixture Model, with the DRC saturating at a different dose level for each group. In order to establish a common DRC, or SGC, for each group, we propose a new normalisation method, the so-called least-squares normalisation procedure (‘LS-normalisation’), which largely reduces the variation between aliquots within the same group and allows the establishment of a common DRC, or SGC, for each group. In order to apply the SGC method for these samples, two regenerative dose points are needed for each aliquot to attribute it to one of the groups based on the ratio of the L_x/T_x signals for two sensitivity-corrected regenerative dose points. Equivalent dose (D_e) values for each aliquot can be estimated using the fitting parameters calculated for the SGC of the relevant group to which it belongs, together with measurements of the natural signal (L_n), one regenerative dose signal (L_x1) and their corresponding test dose signals (T_n, T_x1). For the samples investigated from Haua Fteah, we found that D_e estimates obtained from the SGCs are consistent with those obtained using a full SAR procedure. Our results suggest that small single-aliquot and single-grain D_e values obtained from application of the SGC may be underestimated if there is a significant proportion of early-saturating grains present in the sample; such grains or aliquots are mostly rejected due to saturation when analysed using the full SAR procedure. In this case, it is necessary to calculate the D_e values based only on those grains or aliquots that have relatively high saturation levels.     

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.     

Potential of establishing a ‘global standardised growth curve’ (gSGC) for optical dating of quartz from sediments

We report investigations of the optically stimulated luminescence (OSL) signals of sedimentary quartz from different regions of Asia, Africa, Europe and North America using a single-aliquot regenerative-dose (SAR) procedure. We show that variations in the shape of dose response curves (DRCs), or growth curves, of the test dose sensitivity-corrected OSL signals among single aliquots composed of multiple grains can be greatly reduced by normalising the DRCs using one of the regenerative dose OSL signals. We refer to this regenerative-dose normalisation procedure as ‘re-normalisation’. We find a common re-normalised DRC extends to doses of ∼250 Gy for samples that differ significantly in terms of geological provenance, sedimentary context and depositional age. This feature permits the development of a ‘global standardised growth curve’ (gSGC) for OSL signals from single aliquots of quartz. The equivalent dose (D_e) of an aliquot can be estimated from the natural signal, one regenerative dose signal and their corresponding test dose signals. For the variety of samples investigated, we find that D_e estimates obtained from the gSGC are consistent with those obtained using full SAR procedures for doses of up to ∼250 Gy. Use of the gSGC for single aliquots would greatly reduce the time required to estimate the D_e values of older samples and for a large number of aliquots.     

Construction of a ‘global standardised growth curve’ (gSGC) for infrared stimulated luminescence dating of K-feldspar

We investigated the infrared stimulated luminescence (IRSL) and post-infrared IRSL (pIRIR) signals emitted by K-feldspars from sedimentary samples from Asia, Europe and Africa using a single-aliquot multiple elevated temperature (MET) stimulation procedure. For separate aliquots of the same sample, we show that variation among the dose response curves (DRCs), or growth curves, constructed from the regenerative dose signal (L_x), the test dose signal (T_x, an indicator of luminescence sensitivity) and the sensitivity-corrected signal (L_x/T_x) can be largely eliminated by normalising the DRCs using one of the regenerative dose signals; we call this procedure ‘regenerative-dose normalisation’ or re-normalisation. Furthermore, for the MET-pIRIR signals measured at 250 °C, we find that different samples have re-normalised DRCs that follow the same growth function, despite the samples differing significantly in terms of their geological provenance, sedimentary context, equivalent dose (D_e) and luminescence sensitivity. This common feature offers the potential to establish a ‘global standardised growth curve’ (gSGC) for different samples of K-feldspar, and thereby enable D_e values to be estimated for a large number of single aliquots by projecting the re-normalised natural signals on to the gSGC. For the 18 samples investigated in this study, we find that D_e estimates obtained from the gSGC are consistent with those obtained using full single-aliquot regenerative dose (SAR) procedures for doses of up to ∼1600 Gy. The establishment of a gSGC would greatly reduce the time required to date older samples using K-feldspar, as regenerative doses of several hundreds to a few thousands of Gy are typically delivered to each aliquot in each SAR cycle.     

Stochastic modelling of multi-grain equivalent dose (De) distributions: Implications for OSL dating of sediment mixtures

A number of recent optically stimulated luminescence (OSL) studies have cited post-depositional mixing as a dominant source of equivalent dose (D_e) scatter across a range of sedimentary environments, including those previously considered ‘best suited’ for OSL dating. The potentially insidious nature of sediment mixing means that this problem may often only be identifiable by careful statistical analysis of D_e data sets. This study aims to address some of the important issues associated with the characterisation and statistical treatment of mixed D_e distributions at the multi-grain scale of analysis, using simulated D_e data sets produced with a simple stochastic model. Using this Monte Carlo approach we were able to generate theoretical distributions of single-grain D_e values, which were then randomly mixed together to simulate multi-grain aliquot D_e distributions containing a known number of mixing components and known corresponding burial doses. A range of sensitivity tests were undertaken using sediment mixtures with different aged dose components, different numbers of mixing components, and different types of dose component distributions (fully bleached, heterogeneously bleached and significantly overdispersed D_e distributions). The results of our modelling simulations reveal the inherent problems encountered when dating mixed sedimentary samples with multi-grain D_e estimation techniques. ‘Phantom’ dose components (i.e. discrete dose populations that do not correspond to the original single-grain mixing components) are an inevitable consequence of the ‘averaging’ effects of multi-grain D_e analysis, and prevent the correct number of mixing components being identified with the finite mixture model (FMM) for all of the multi-grain mixtures tested. Our findings caution against use of the FMM for multi-grain aliquot D_e data sets, even when the aliquots consist of only a few grains.     

Variability in quartz OSL signals caused by measurement uncertainties: Problems and solutions

We simulated the variability in measured quartz optically stimulated luminescence (OSL) signals and dose response curves (DRCs) caused by measurement uncertainties, including counting statistics and instrumental irreproducibility. We find that these measurement errors can give rise to large variations in the observed luminescence signal and contribute to among-aliquot or among-grain scatter in DRCs and equivalent dose (D_e) values. Different measurement systems (i.e., luminescence readers) may have different counting statistics properties and, hence, may exhibit differing extents of variation in the observed OSL signal, even for the same sample. Our simulation shows that the random measurement uncertainties may result in some grains or aliquots being ‘saturated’ (that is, the measured natural signal is consistent with, or lies above, the saturation level of the measured DRC) and that the rejection of these ‘saturated’ grains may result in a truncated D_e distribution, with D_e underestimation for samples with natural doses close to saturation (e.g., twice the characteristic saturation dose, D₀). We propose a new method to deal with this underestimation problem, in which standardised growth curves (SGCs) are established and the weighted-mean natural signal (L_n/T_n) from all measured grains is projected on to the corresponding SGCs to determine D_e. Our simulation results show that this method can produce reliable D_e estimates up to 5D₀, which is far beyond the conventional limit of ∼2D₀ using the standard SAR procedure.     

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.     

OSL dating of loess deposits bracketing Sheep Creek tephra beds,northwest Canada: Dim and problematic single-grain OSL characteristics and their effect on multi-grain age estimates

Geochemically-fingerprinted tephra beds provide unique chronostratigraphic markers for comparing Quaternary sedimentary records across eastern Beringia (Alaska and Yukon Territory). Establishing reliable numerical age control on these tephra horizons enables them to be placed within firm temporal frameworks and increases their potential as correlative tools for regional palaeoenvironmental reconstructions. To this end we present new single-grain and multi-grain quartz optically stimulated luminescence (OSL) chronologies for loess deposits bracketing three well-documented and regionally significant variants of the Sheep Creek tephra (SCt) at two sites in west-central Yukon Territory (Ash Bend and Quartz Creek). Single-grain OSL ages bracketing the SCt-A and SCt-K reveal that these tephras were deposited during late Marine Isotope Stage (MIS) 5 or early MIS 4. The SCt-C variant and associated organic-rich bed at Ash Bend were likely deposited during late MIS 5, based on a single-grain OSL age of ∼81 ka for the overlying sediments. The single-grain OSL ages obtained for these deposits are in stratigraphic order and in broad agreement with a fission track age estimate of ∼77 ka for the SCt-K. In contrast, comparative chronologies obtained using multi-grain aliquots are stratigraphically inconsistent and unexpectedly young when compared with the independent SCt-K age. Detailed examination of the single-grain OSL datasets reveal a range of unfavourable luminescent properties that could have contributed to the multi-grain aliquot age discrepancies; including, very low yields of luminescent grains, weak OSL signal sensitivities and large populations of aberrant grains (particularly 0 Gy grains and ‘dim’ grains with a tendency to sensitise during the equivalent dose (D_e) measurement sequence) that have similarly sized OSL signals as grains used for D_e analysis. Synthetic aliquot D_e datasets constructed from single-grain OSL measurements reveal that the large proportional light sum contributions of 0 Gy and dim grains could possibly account for multi-grain age underestimations in some of the Ash Bend samples. In light of these potentially problematic averaging effects, we do not consider the multi-grain OSL ages to be reliable and suggest that single-grain approaches may be preferable for dating sediments with similar quartz luminescence behaviours across this region.     

Investigating the potential of HCl-only treated samples using range-finder OSL dating

Rapid sample preparation and measurement protocols for optically stimulated luminescence (OSL) dating have been investigated as a method of increasing the throughput of samples (e.g. Roberts et al. 2009). Here, we investigate the potential of dating samples treated using only hydrochloric acid (HCl) for providing accurate range-finder ages for quartz. The equivalent dose (D_e) is underestimated for older samples using a standard single-aliquot regenerative-dose (SAR) protocol, but measurement of the post-IR OSL signal (e.g. Roberts and Wintle, 2003) provides D_e estimates within 15% of the ‘target fully prepared D_e’ for two-thirds of samples. The application of a standardised growth curve (SGC) is also investigated. For these dune samples, the most efficient preparation and measurement procedure from which accurate D_e estimates can be obtained is treatment with HCl-only, measurement of the natural and regenerative post-IR OSL signal, and calculation using a region-independent SGC. A slightly longer protocol incorporating an additional preparation stage of heavy liquid density separation can be used to improve D_e estimates in samples where feldspar-contamination is thought to be particularly problematic. In practice, these time savings of days to weeks in the preparation and measurement protocols mean that a large number of samples can first be rapidly treated with HCl, the post-IR blue OSL signal measured using a shortened double-SAR protocol, and D_e calculated by applying an independent SGC before then deciding which samples require full preparation and measurement, rather than the inefficiency of committing time and resources to all samples if this is unnecessary for the context of a particular suite of samples. The potential of this rapid preparation and measurement protocol is discussed in relation to sand dune dating studies.     

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.     

Statistical aspects of equivalent dose and error calculation and display in OSL dating: An overview and some recommendations

All Quaternary dating methods involve the measurement of one or more variables to estimate the age of a sample. Each measured quantity has an associated error and uncertainty, and may also be subject to natural variation. We review the statistical estimation of such uncertainties and variation for comparing and interpreting age estimates, with specific reference to the estimation of equivalent dose (D_e) values in the optically stimulated luminescence (OSL) dating of sediments. We discuss statistical aspects of OSL signal and background estimation, the determination of D_e values for multi-grain aliquots and individual mineral grains from the same and different samples, and the extent of variation commonly observed among such estimates. Examples are drawn from geological and archaeological contexts. We discuss the strengths and weaknesses of various graphical methods of displaying multiple, independent estimates of D_e, along with statistical tests and models to compare and appropriately combine them. Many of our recommendations are applicable also to the clear presentation of data obtained using other Quaternary dating methods. We encourage the use of models and methods that are based on well established statistical principles and, ideally, are validated by appropriate numerical simulations; and we discourage the adoption of ad hoc methods developed using a particular set of measurement conditions and tested on a limited number of samples, as these may not be applicable more generally. We emphasise that the choice of statistical models should not be made solely on statistical grounds (or arbitrary rules) but should take into account the broader scientific context of each sample and any additional pertinent information.     

OSL and IRSL dating of raised beach sand deposits along the southeastern coast of Norway

Raised beach sand deposits along the southeastern coast of Norway were dated by optical (OSL) and infrared stimulated luminescence (IRSL) and the quartz and K-feldspar luminescence characteristics were described. Due to the poor quartz luminescence characteristics, only a limited number of samples were suitable for OSL dating. More promising are the K-feldspar extracts, with typical K-feldspar luminescence characteristics and no sign of fading. For equivalent dose (D_e) determination, sand-size quartz and feldspar extracts were used, applying a single aliquot regenerative (SAR) protocol. Both, OSL and IRSL D_e estimates show a wide distribution, unexpected for beach deposits. The calculated OSL and IRSL age estimates were generally in good agreement and the correctness of the ages was confirmed by independent age control. Because only a limited number of the quartz samples were suitable for OSL dating, IRSL dating of the K-feldspar represents an alternative to OSL quartz dating.     

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.     

Optically stimulated luminescence dating of single and multiple grains of quartz from perennially frozen loess in western Yukon Territory, Canada: Comparison with radiocarbon chronologies for the late Pleistocene Dawson tephra

Optically stimulated luminescence (OSL) dating of perennially frozen loess was tested on quartz grains extracted from deposits associated with the late Pleistocene Dawson tephra in western Yukon Territory, Canada. OSL samples were obtained from ice-rich loess bracketing the Dawson tephra, while radiocarbon (¹⁴C) samples were collected from the bulk sediments directly underlying the tephra and from a ground-squirrel burrow 2.7 m below the tephra. Here we report the OSL characteristics and ages of the extracted quartz grains, as well as additional radiocarbon ages for samples described in Froese [2002. Age and significance of the late Pleistocene Dawson tephra in eastern Beringia. Quaternary Science Reviews 21, 2137–2142; 2006. Seasonality of the late Pleistocene Dawson tephra and exceptional preservation of a buried riparian surface in central Yukon Territory, Canada. Quaternary Science Reviews 25, 1542–1551]. We refine the time of Dawson tephra deposition to between 25,420±70 and 25,290±80 ¹⁴C a BP. Bayesian analysis of constraining radiocarbon ages places the deposition of the Dawson tephra at between 30,433 and 30,032 cal a BP. Linear modulation (LM) OSL analysis of multi-grain aliquots of quartz showed that the initial part of the decay curve is dominated by a rapidly bleached (‘fast’) component; these samples, however, had relatively dim continuous wave (CW) OSL signals at the multi-grain aliquot (each composed of 80 grains) and single-grain scales of analysis. The single-aliquot regenerative-dose protocol was applied to multi-grain aliquots and single grains to obtain equivalent dose (D_e) values for samples collected from below and above the Dawson tephra. The D_e values were examined graphically and numerically, the latter using the central age, minimum age, and finite mixture models. For multi-grain aliquots, the central age model gave weighted mean D_e values between 30 and 50 Gy, which greatly underestimated the expected D_e of 74–81 Gy for both samples studied. Possible reasons for these underestimations are discussed, and a solution proposed based on single-grain analysis. Measurements of single grains produced D_e values in agreement with the expected D_e, and yielded OSL ages of 28±5 and 30±4 ka for the samples taken from above and below the Dawson tephra, respectively. Examination of individual grains with differing luminescence behaviors showed that a significant number of the measured quartz grains exhibited anomalous luminescence properties that would have compromised the results obtained from multi-grain aliquots. We therefore recommend analysis of individual grains to overcome the age-shortfall from multi-grain analysis of these and similar samples of quartz.     

Testing the applicability of a standardized growth curve (SGC) for quartz OSL dating: Kalahari dunes,South African coastal dunes and Florida dune cordons

Standardized growth curves (SGCs) have recently been developed as a means to reduce measurement times when determining palaeodoses in the standardized luminescence (OSL) dating of quartz, but this approach is not without its critics. We test the performance of SGCs derived from samples from a range of environments in southern Africa and Florida (United States of America). Data presented here suggest that the method performed well when determining low (<50 Gy) equivalent dose (D_e) values from samples with different geological provenances within South Africa. However, the application of an SGC built from South African data performed poorly when used to estimate the palaeodoses of samples from Florida, with seven out of ten samples failing to replicate the single aliquot regenerative (SAR)-derived D_e value to within ±10%. We thus advocate the use only of regionally based SGCs for full D_e determination, although SGCs can also be utilized as a way of quickly generating SAR ‘range finders’ irrespective of sample origin. Furthermore, one sample from the Florida site did not show regenerative growth in accordance with any samples from either the South Africa or Florida data, resulting in significant D_e underestimation when using the SGC. Although the reasons for such behaviour are not yet understood, this re-iterates the recommendation of Burbidge et al. [2006. D_e determination for young samples using the standardised OSL response of coarse-grain quartz. Radiation Measurements 41(3), 278], to incorporate a single regenerative step in SGC protocols in order to check consistency.     

The source of De variability in periglacial sand wedges: Depositional processes versus measurement issues

Relict periglacial wedge structures are widespread in mid-latitude and polar regions. The wedges have a high preservation potential and are often infilled with quartz-rich aeolian sand, making them potentially suitable for luminescence dating. This paper presents initial work from an anti-syngenetic sand wedge in the Tuktoyaktuk Coastlands, Arctic Canada. When samples were measured at the single grain level they showed poor palaeodose (D_e) reproducibility and consequent high age uncertainties. The aim of the study was to determine whether this intra-sample D_e scatter reflected methodological issues arising from OSL measurement or processes of wedge development.Initial single grain dose recovery tests show that D_e scatter was not easily explained by poor recycling, sensitivity changes, variable OSL components, recuperation problems, or large D_e uncertainties from dim grains. Single grain preheating tests did show that some D_e scatter might be attributable to individual grains requiring different preheat temperatures, whilst dose recovery tests revealed that highly sensitive grains showed less scatter than dim grains. However, selection of these bright grains from natural samples still resulted in scattered D_e values. An alternative explanation for the D_e scatter relates to the formation of anti-syngenetic sand wedges by thermal contraction cracking over thousands of years in an eroding landscape, which may result in sediment of very different ages being deposited in adjacent cracks. Finite mixture modelling was used to identify D_e components within each sample. Ages calculated from these components suggest sand wedge formation at ca. 5, 8.5, 12.5 and 18 ka which correlate well with known cooling events over the last 18 ka and support a multiple phase activity model for anti-syngenetic sand wedges.     

Insights into TT-OSL signal stability from single-grain analyses of known-age deposits at Atapuerca,Spain

Single-grain thermally transferred optically stimulated luminescence (TT-OSL) dating has recently been applied to a number of the Atapuerca palaeoanthropological sites. As yet, however, there have not been any direct assessments of TT-OSL signal stabilities for specific grains used for dating. In this study, we undertake a series of TT-OSL suitability assessments on known-age samples from Gran Dolina and Sima del Elefante. Our results suggest that the Atapuerca samples contain populations or sub-populations of grains with suitably stable TT-OSL signals for dating over late-Early and Middle Pleistocene timescales. Equivalent dose (D_e) distribution analysis in combination with pulse-annealing assessments provides a useful means of identifying inter-grain and inter-sample differences in TT-OSL signal stabilities. We also show that obtaining D_e values using different preheat conditions may help to identify potentially problematic TT-OSL behaviours. Analyses of multi-grain aliquot TL curves for these samples reveal that 'bulk' TL signal loss experiments may provide limited insights into TT-OSL source trap lifetimes due to averaging effects, the dominance of grain populations that do not produce TT-OSL, and interference from slowly bleaching OSL components. Our results improve the robustness and precision of existing TT-OSL chronologies for units TD6-3 and TE16-TE17 at Gran Dolina and Sima del Elefante, and support the broader suitability of the single-grain TT-OSL approach at the Atapuerca sites.     

Modelling dose rate to single grains of quartz in well-sorted sand samples: The dispersion arising from the presence of potassium feldspars and implications for single grain OSL dating

Single grain OSL has become a widely used approach in Quaternary geochronology. However, the origins of D_e distributions and the sources of variation in individual dose estimates are still poorly understood. The amount of scatter in these distributions on top of the known uncertainties in measurement and analysis is defined by overdispersion and this quantity is generally used for weighting individual D_e values to calculate a central equivalent dose. In this study, we address the nature and amount of different sources of dispersion in quartz single grain D_e estimates, by (i) using appropriate statistical tools to characterize D_e populations and (ii) modelling, with a specifically designed Geant4 code, dose rate distributions arising from the presence of potassium feldspar grains in well-sorted sands. The model uses Monte Carlo simulations of beta emissions and interactions in a random close packing of quartz and feldspar spheres representing a sand sample. Based on the simulation results, we explain the discrepancy between intrinsic and natural overdispersion values in a well-bleached sample, thus validating the model. The three parameters having the most influence on dispersion in dose rate distributions, and modelled in this study, appear to be grain size, potassium content and total dose rate.Finally an analysis of measurement uncertainties and other sources of variations in equivalent dose estimates lead us to conclude that all age models (both logged and unlogged) which include an overdispersion value to weight individual D_e values rely mainly on unknown parameters; this ignorance may lead to an inadvertent bias in D_e estimates. Assuming counting statistics make a small contribution to dispersion (as is often the case), we suggest that in some cases it is most appropriate to use unweighted averages of equivalent doses when dividing by commonly measured average dose rates.     

Maximum age limitation in luminescence dating of Chinese loess using the multiple-aliquot MET-pIRIR signals from K-feldspar

Numerical dating of loess is important for Quaternary studies. Recent progress in post-infrared infrared-stimulated luminescence (pIRIR) signals from potassium-rich feldspar has allowed successful dating of Chinese loess beyond the conventional dating limit based on quartz optically stimulated luminescence (OSL) signals. In this study we tested the multiple-aliquot regenerative-dose (MAR) pre-dose multiple-elevated-temperature post-IR IRSL (pMET-pIRIR) procedure on samples from the palaeosol S5 (∼480 ka) and S8 (∼780 ka) layers from the Luochuan and Jingbian sections, respectively. The results show that (1) compared to sensitivity-corrected signal (L_x/T_x), a higher saturation dose is observed for the sensitivity-uncorrected MET-pIRIR signals (L_x), suggesting that MAR is advantageous for dating old samples; (2) negligible fading component can be achieved using the pMET-pIRIR procedure; (3) for the sample from the top of palaeosol S5, D_e values (1360 + 226/-167 Gy) broadly consistent with expected D_e (1550 ± 72 Gy) can be obtained using the sensitivity-uncorrected 300 °C MET-pIRIR signal. Our study suggests that a D_e value of about 1800 Gy may be the maximum dating limit of Chinese loess using the MAR pMET-pIRIR procedure.     

Electron spin resonance dating of optically bleached quartz grains from the Middle Palaeolithic site of Cuesta de la Bajada (Spain) using the multiple centres approach

Electron spin resonance (ESR) dating of optically bleached quartz grains was performed on three sediment samples collected from the Middle Palaeolithic site of Cuesta de la Bajada (Spain). A standard multiple grain and multiple aliquot additive dose procedure was employed, and both the Al and Ti centres were measured as part of the multiple centres approach.ESR age estimates obtained for the three samples indicate that the Al centre provides a maximum possible chronology, as the Ti centres show that the Al signal was likely not systematically reset to its residual level during sediment transport. A direct comparison between ESR ages based on the Ti centres and single grain optically stimulated luminescence (OSL) ages from samples collected nearby shows broadly consistent results. The Ti-H centre also appears to provide suitable chronologies for at least two of the three Middle Pleistocene samples studied here. Surprisingly, the only sample showing consistent ESR ages between the Al and Ti centres appears to be overestimated in comparison with the Ti-centre and OSL ages derived from the other two samples. This indicates either incomplete bleaching of both the Al and Ti centres for this sample, or unexpected impacts of other sources of D_e uncertainty, such as multi-grain averaging effects. The ESR dating results overall indicate that the archaeological sequence of Cuesta de la Bajada CB-3 is most likely correlated to either MIS 7 or 9.