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.     

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.     

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.     

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.     

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.     

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.     

Bayesian analysis of De distributions in optical dating: Towards a robust method for dealing with outliers

In optical dating, especially single-grain dating, various patterns of distributions in equivalent dose (D_e) are usually observed and analysed using different statistical models. None of these methods, however, is designed to deal with outliers that do not form part of the population of grains associated with the event of interest (the ‘target population’), despite outliers being commonly present in single-grain D_e distributions. In this paper, we present a Bayesian method for detecting D_e outliers and making allowance for them when estimating the D_e value of the target population. We test this so-called Bayesian outlier model (BOM) using data sets obtained for individual grains of quartz from sediments deposited in a variety of settings, and in simulations. We find that the BOM is suitable for single-grain D_e distributions containing outliers that, for a variety of reasons, do not form part of the target population. For example, D_e outliers may be associated with grains that have undesirable luminescence properties (e.g., thermal instability, high rates of anomalous fading) or with contaminant grains incorporated into a sample when collected in the field or prepared in the laboratory. Grains that have much larger or smaller D_e values than the target population, due to factors such as insufficient bleaching, beta-dose heterogeneity or post-depositional disturbance, may also be identified as outliers using the BOM, enabling these values to be weighted appropriately for final D_e and age determination.     

Potential of quartz OSL dating on moraine deposits from eastern Tibetan Plateau using SAR protocol

Optically stimulated luminescence (OSL) dating methods have been widely applied in Quaternary glaciology. However, glacigenic deposits are considered in general as problematic for OSL dating, mainly because they are transported shorter distances prior to burial and are usually partially bleached. Thus, most researchers choose glaciofluvial and glaciolacustrine sediments (with relatively longer transportation times) for OSL dating when constraining the age of glaciation. In this study, four samples were collected from a lateral moraine series at Zhuqing Village, northern margin of Queer Shan Mountain, eastern Tibetan Plateau, in order to investigate the applicability of OSL dating for morainic deposits. Quartz grains (38–63 μm) were extracted and measured using single aliquot regenerative-dose (SAR) protocol. Internal checks and dose recovery test show that the SAR protocol is appropriate for equivalent dose (D_e) determination. The effect of thermal transfer is small for all samples and the recycling ratio for each individual sample is close to unity. The symmetry in the D_e distributions indicates that quartz grains were well-bleached prior to burial. OSL ages show good agreement with geomorphological and field investigations, and are also concordant with an independent ESR age. It is concluded that: (a) the morainic deposits in Zhuqing were well-bleached and suitable for OSL dating; (b) SAR protocol can be applied to morainic deposits for samples under study.     

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.     

OSL dating of mixed coastal sediment (Sylt,German Bight,North Sea)

As part of a study on coastal sedimentary processes this paper presents the OSL dating of mixed coastal sediment samples from the southern North Sea island of Sylt (German Bight). During coring of the swash-bar (beach) sediments, five samples were presumably contaminated by younger overwash and aeolian sediments because of the sampling method employed. To obtain reliable burial ages for these swash-bar sediments, single-grain and small aliquot measurements were used together with the Finite Mixture Model (FMM) proposed by Roberts et al. (2000) to identify the grain population containing the largest doses (from the deepest part of the core). Before the FMM was applied to dating, the parameters and performance of the FMM were first investigated by systematically comparing small aliquot (∼20 grains) and single-grain measurements of an undisturbed aeolian and swash-bar sample and a laboratory mixture of both sediments. This test case demonstrates the advantage of selecting the time interval immediately following the initial luminescence signals for background subtraction because unsuitable quartz grains were removed from the dose distribution. It is concluded that the measurement of small aliquots can be regarded as a reliable proxy for single-grain dose distribution if the sediment contains only a small proportion of quartz grains emitting a luminescence signal and that the FMM results are relatively insensitive to changes of the over-dispersion parameter between 5–40% for small aliquots and 10–40% for single-grains.We show that the burial ages of the contaminated swash-bar samples resulting from the maximum age populations from equivalent dose distributions measured using small aliquots are consistent with the stratigraphy and with ages obtained from uncontaminated samples.     

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.     

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.     

Single-grain dating of young sediments using the pIRIR signal from feldspar

In this article we test for the first time the potential of single-grains of K-rich feldspar to date well-bleached and poorly bleached sediments using a post-IR IRSL (pIRIR) protocol. We measure natural dose distributions using K-rich feldspars from four coastal samples applying the pIRIR protocol with a preheat of 200 °C and a pIRIR stimulation temperature of 180 °C; each sample had an independent age control obtained from quartz OSL and radiocarbon dating. We also analyse single-grain dose distributions of “zero-dose” and γ-irradiated samples to determine thermal transfer/residual doses and the intrinsic sources of variability of pIRIR single-grain measurements, respectively. Based on these experiments, we conclude that thermal transfer/residual dose give rise to an offset of ∼0.6 Gy in these samples and that the uncertainty assigned to individual pIRIR single-grain dose estimates cannot be smaller than 16.5%.The analysis of the well-bleached samples shows that only the brightest 30% of the grains give pIRIR single-grain ages in agreement with the age control; this effect may arise from the suggested correlation between blue emission and potassium content of individual grains. Comparison of single-grain quartz and feldspar dose distributions from the poorly bleached samples shows that quartz is relatively better bleached; nevertheless, selection of a reliable ‘minimum’ feldspar dose was achieved using two different statistical models.     

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.     

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.     

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.     

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.     

Testing single-grain quartz OSL methods using sediment samples with independent age control from the Bordes-Fitte rockshelter (Roches d'Abilly site,Central France)

We present quartz single-grain dose distributions for four well-bleached and unmixed sediment samples with independent age control (22–48 ka), from the archaeologically important Bordes-Fitte rockshelter at Roches d'Abilly, France. This site has previously been dated using ¹⁴C AMS dating and standard multi-grain OSL dating using both quartz and feldspar. The effect of rejection criteria usually employed in single-grain dating on dose and over-dispersion is tested using both laboratory irradiated samples and natural samples. It is shown that had these samples been analysed in the absence of other age control, standard modelling decisions based on the shape of single-grain dose distributions would have led to significant misinterpretation of results and a corresponding >40% underestimation in age. If we instead ignore this standard decision process and apply weighted average and mixing models then the most likely results deviate from the expected ages by >10%. Finally, we show that by careful consideration of the luminescence characteristics of individual grains, we are able to obtain good agreement with the independent age control by applying alternative rejection criteria but this is at the cost of reducing the accepted grain population by more than an order of magnitude, with the corresponding inevitable decrease in precision.     

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.     

Optical dating of young deltaic deposits on a decadal time scale

Modern Mississippi Delta sediments were analyzed to investigate quartz OSL signal resetting in large river deltas and test the accuracy of OSL dating on a decadal time scale with the early background subtraction and a recently proposed burial dose estimation procedure. Both fine silt-sized and sand-sized quartz were measured with a modified single-aliquot regenerative dose (SAR) protocol and equivalent dose (D_e) was calculated using different background subtraction methods. Evidence of insufficient bleaching was observed, but the residual signal is equivalent to ∼100 a on average for both sandy quartz and fine silt-sized quartz. It is shown that dose distributions of sandy quartz are affected by the background subtraction. The proportion of aliquots that have D_e in agreement with expectation is significantly larger when an early background is subtracted compared to the late background subtraction. This is, in contrast, not observed for fine silt-sized quartz. Accurate OSL ages were obtained by employing the unlogged minimum age model to D_es of sandy quartz obtained with the early background subtraction method.