Single grain optically stimulated luminescence dating of glacial sediments from the Baiyu Valley,southeastern Tibet

The Qinghai-Tibetan Plateau is an important area for the study of Quaternary glaciation. Optically stimulated luminescence (OSL) dating has the potential to contribute to the chronology of glaciation in this region, but it is important to assess the accuracy of OSL dating of these glacial sediments. In this study, single grain quartz OSL signals are examined for five glacial samples collected from the moraines outside the Baiyu Valley, southeastern Tibet. The quartz grains exhibit poor luminescence characteristics, with a small proportion of grains passing the screening criteria. Grains which pass the screening criteria have relatively low signal intensity, leading to D_e values with large uncertainties. MAM and CAM were used to determine D_e values for these samples. The OSL ages are consistent with the sequence of events derived from the geomorphological relationship of the samples, and also with previous published radiocarbon ages. However, it is more difficult to reconcile the OSL ages and the terrestrial cosmogenic nuclide (TCN) ¹⁰Be ages. Analysis of both single grain quartz OSL data and TCN ¹⁰Be data is complex in this area. Further work is required to increase confidence in the OSL ages generated for the glacial sediments from this region.     

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.     

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.     

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.     

Comparison of paired quartz OSL and feldspar post-IR IRSL dose distributions in poorly bleached fluvial sediments from South Africa

A comparative study using quartz optically stimulated luminescence (OSL) and feldspar post-infrared infrared stimulated luminescence (post-IR IRSL) was undertaken on Quaternary fluvial sediments from an unnamed tributary of the Moopetsi River in South Africa. The aim is to assess whether the post-IR IRSL signal can be used to date incompletely bleached sediments. Several post-IR IRSL signals using varying stimulation and preheat temperatures were investigated; of these the post-IR IRSL₂₂₅ signal was deemed most appropriate for dating because it bleached most rapidly. The feldspar post-IR IRSL₂₂₅ equivalent dose (D_e) values from this site are consistently larger than those from quartz OSL, probably due to differences in the bleaching characteristics of the two signals. Additionally, the post-IR IRSL₂₂₅ D_e values within a sample showed less variation in precision than the quartz D_e data, possibly due to greater averaging between grains in the feldspar small aliquots. The agreement between ages based on the OSL and post-IR IRSL₂₂₅ signals was better for younger samples (<20 ka) than for older ones (>50 ka); the cause of this variation is unclear.     

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.     

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.     

OSL chronostratigraphy of a loess-palaeosol sequence in Saxony/Germany using quartz of different grain sizes

Luminescence dating is one of the leading techniques to establish chronologies for loess-palaeosol sequences and has been successfully applied to different minerals and grain size fractions. Using optical stimulated luminescence (OSL) from quartz, we present for the first time a high resolution chronology for the loess section Ostrau in Saxony/Germany. We compare OSL ages derived from two different grain size fractions, coarse (90–200 μm) and the fine grain (4–11 μm) separates. Our results show that the loess section is divided into two parts, separated by a hiatus. OSL samples from the upper part of the loess section show equivalent doses of D_e < 100 Gy. D_e values >180 Gy are observed for the lower part of the loess section. The coarse and fine grain ages agree and also fit to the litho- and pedostratigraphy for the upper part of the profile. For the lower part of the profile the coarse grained quartz OSL is in saturation. The fine grained quartz OSL is not saturated but it appears that the fine grain OSL ages underestimate the sedimentation age. Approaches to explain the D_e differences between the grain size fractions are presented (e.g. post-depositional translocation, dosimetry). A modified SAR protocol for the fine grain fraction produced ages that are in good agreement with expected ages based on litho- and pedostratigraphy. Although further investigations are needed, our results show the suitability of the Saxonian loess belt for OSL dating.     

Rapid equivalent dose estimation for eolian dune sands using a portable OSL reader and polymineralic standardised luminescence growth curves: Expedited sample screening for OSL dating

Portable optically stimulated luminescence (OSL) readers are robust devices that allow rapid determination of luminescence signals of polymineralic coarse-grained samples. To date, however, the utility of portable OSL readers has largely been confined to the construction of luminescence profiles that depict variations of luminescence signal intensities with depth. Because the luminescence signals used to construct such profiles are uncalibrated, it is neither practical to quantitatively compare portable OSL data from different sites nor is it possible to approximate sample ages. Such comparisons could be facilitated by converting portable OSL signals into equivalent doses (D_e). However, determining D_e requires the construction of unique growth curves for each sample; a laborious procedure that negates the rapidity associated with portable measurements. To circumvent that limitation, we construct standardised growth curves (SGCs) using normalized regeneration dose signals obtained using a portable OSL reader from the feldspar component of polymineralic sands from five disparate eolian dune sites in Alberta, Canada. Comparison of SGCs from different samples indicates general congruence and we merge these to construct a regionally applicable curve which we test by comparing the D_e obtained from given samples with that obtained using conventional OSL dating protocols. Results show that, though the uncertainties associated with the portable OSL data are high, the D_e values from the two approaches are linearly proportional. This direct variation enables portable OSL SGC D_e values to be used independently in reconnaissance studies that aim to screen samples for more detailed analysis using standard OSL methods. The affordability of portable OSL readers suggests that the approach could be attractive to researchers who do not have ready access to conventional OSL readers.     

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.     

Luminescence dating of K-feldspar from sediments: A protocol without anomalous fading correction

A protocol for optical dating of potassium-rich feldspar (K-feldspar) is proposed. It utilizes the infrared stimulated luminescence (IRSL) signal measured by progressively increasing the stimulation temperature from 50 to 250 °C in step of 50 °C, so-called multi-elevated-temperature post-IR IRSL (MET-pIRIR) measurements. Negligible anomalous fading was observed for the MET-pIRIR signals obtained at 200 and 250 °C. This was supported by equivalent dose (D_e) measurements using the IRSL and MET-pIRIR signals. The D_e values increase progressively from 50 °C to 200 °C, but similar D_e values were obtained for the MET-pIRIR signal at 200 and 250 °C. Measurement of modern samples and bleached samples indicates that the MET-pIRIR signals have small residual doses less than 5 Gy equivalent to about 1–2 ka. We have tested the protocol using various sedimentary samples with different ages from different regions of China. The MET-pIR IRSL ages obtained at 200 and 250 °C are consistent with independent and/or quartz OSL ages.     

Infrared stimulated luminescence and radiofluorescence dating of aeolian sediments from Hungary

Anomalous fading of the infrared stimulated luminescence (IRSL) signal from the polymineral fine-grain and K-feldspar fractions of aeolian sediments from Hungary has been studied. The samples in this study have previously been dated using the multiple aliquot additive dose (MAAD) protocol to measure the IRSL signal. The IRSL measurements using MAAD were conducted ～4 weeks after the irradiation, making it difficult to assess to what extent these age estimates were affected by anomalous fading. In this study, equivalent doses were obtained using the single aliquot regenerative dose (SAR) protocol. The fading rate for each sample was calculated using the different IRSL components and different parts of the decay curve. For each sample, the middle part of the decay curve always showed a lower fading rate than the initial part of the decay curve. The difference between the fading rates for different parts of the decay curve was greater for the K-feldspars than for the polymineral fine grains. Fading corrected ages were calculated by integrating both the initial and the middle part of the decay curve. These ages were compared with optically stimulated luminescence (OSL) ages from quartz, infrared radiofluorescence (IR-RF) ages obtained from K-feldspars and also with independent ages, provided by radiocarbon dating of shells and charcoal, and uranium-series dating of travertine.     

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.     

Direct measurement of the fast component of quartz optically stimulated luminescence and implications for the accuracy of optical dating

The usual practice in optical dating is to derive an equivalent dose (D_e) (and hence age) from integration of the initial part of the measured optically stimulated luminescence (OSL) signal. This ‘bulk’ OSL signal is known to comprise several semi-independent components, each of which decays at different rates during measurement, and thus contributes a different proportion to the bulk signal as measurement time progresses. Data are presented here which show a strong dependence of D_e on the bulk signal integration interval, with reduced D_e for later signal integration intervals resulting from lower medium component D_e values. This dependence leads to two problems: (i) deciding which signal integral to choose, and (ii) the possibility that all bulk signals will provide systematic age underestimation due to medium component signal contributions. Isolating the fast component of the bulk OSL signal provides a solution to both problems and several methods of achieving this are assessed; an efficient new method is described which is incorporated in to standard single-aliquot regenerative-dose measurement sequences. This method involves the direct measurement of the fast-component signal using infrared (830 nm) stimulation of quartz at 160 °C, prior to the standard bulk OSL measurement with 470 nm stimulation. It is shown that the measured quartz infrared stimulated luminescence signals resolve pure fast-component signals and provide D_e estimates consistent with those from signal deconvolution. This approach can only be applied to samples with relatively bright luminescence emissions, but in these cases is expected to provide a more robust estimate of palaeodose.     

Luminescence dating of quartz from ironstones of the Xingu River,Eastern Amazonia

This study reports on the first investigation into the potential of quartz luminescence dating to establish formation ages of ferruginous duricrust deposits (ironstones) of the Xingu River in Eastern Amazonia, Brazil. The studied ironstones comprise sand and gravel cemented by goethite (FeO(OH)), occurring as sandstones and conglomerates in the riverbed of the Xingu River, a major tributary of the Amazon River. The Xingu ironstones have a cavernous morphology and give origin to particular habitat for benthic biota in an area that hosts the largest rapids in Amazonia. So far, the Xingu ironstones have uncertain formation ages and their sedimentary origin is still poorly understood. In this way, seven samples of ironstones distributed along the lower Xingu River were collected for optically stimulated luminescence (OSL) dating of their detrital quartz sand grains. Additionally, the organic content of some samples was dated by radiocarbon (¹⁴C) for comparison with quartz OSL ages. The luminescence ages of the sand-sized quartz grains extracted from the ironstones were obtained from medium (100–300 grains) and small (10–20 grains) aliquots using the single aliquot regenerative-dose (SAR) protocol. Equivalent doses (D_e) distributions have varied overdispersion (OD) both for medium size aliquots (OD = 19–58 %) and small size aliquots (OD = 29–76 %). No significant trend was observed between D_e and aliquot size. The studied ironstones grow over the riverbed, but stay below or above water throughout the year due to the seasonal water level variation of the Xingu River. However, the effect of water saturation in dose rates is reduced due to relatively low porosity of ironstones. Water saturated dose rates (dry sample dose rates) range from 2.70 ± 0.21 (2.79 ± 0.22) Gy/ka to 12.34 ± 0.97 (13.26 ± 1.12) Gy/ka, which are relatively high when compared to values reported for Brazilian sandy sediments elsewhere (∼1 Gy/ka). Samples with high overdispersion (>40 %) are mainly attributed to mixing of grains trapped in different time periods by goethite cementation. The obtained OSL ages for water saturated (dry) samples range from 3.4 ± 0.3 (3.3 ± 0.4) ka to 59.6 ± 6.0 (58.1 ± 6.4) ka, using D_e determined from medium size aliquots and dose response curves fitted by an exponential plus linear function. Radiocarbon ages of the bulk organic matter extracted from selected ironstone varied from ca. 4 cal ka BP to ca. 23 cal ka BP. Significant differences were observed between OSL and radiocarbon ages, suggesting asynchronous trapping of organic matter and detrital quartz within the ironstone matrix. These late Pleistocene to Holocene ages indicate that ironstones of the Xingu River result from an active surface geochemical system able to precipitate goethite and cement detrital sediments under transport. The obtained ages and differences between OSL and radiocarbon ages point out that the ironstones have multiphase and spatially heterogeneous growth across the Xingu riverbed. Our results also expand the application of luminescence dating to different sedimentary deposits.     

Luminescence dating of scoria fall and lahar deposits from Somma–Vesuvius,Italy

Luminescence dating has been applied to scoria and lahar deposits from Somma–Vesuvius, Italy. Samples include scoria from the AD472 and 512 (or 536) eruptions and lahar deposits. In order to find a stable luminescence signal which is less affected by anomalous fading, infrared stimulated luminescence (IRSL) signals at elevated temperatures after bleaching with IR at 50 °C (termed post-IR IRSL; pIRIR) were tested at different preheat and elevated stimulation temperatures. The fading rates of both IRSL and pIRIR signals reduced dramatically with increasing preheat and pIRIR stimulation temperatures. A pIRIR signal measured at 290 °C after a preheat at 320 °C (60 s) and an IR stimulation at 50 °C (100 s) was selected to calculate the equivalent dose (D_e). The gamma spectrometry results indicate that the U-series nuclides are not in equilibrium and there is a large ²²⁶Ra excess. The dose rates and ages were calculated by assuming a ²²⁶Ra excess (over its parent ²³⁰Th) at deposition, and that this unsupported excess then decayed to the present level. The resulting luminescence ages of the two scoria samples agreed with the expected ages, and the ages of the lahar deposits indicate that they are associated with the AD1631 eruption.     

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.     

Underestimation of fine grain quartz OSL dating towards the Eemian: Comparison with palynostratigraphy from Azzano Decimo,northeastern Italy

Palynostratigraphical records have been used to understand the response of vegetation to climate change, and benefit from independent dating to ensure a robust correlation with global climate and sea-level change. In order to constrain the pollen chronology of a long sedimentary core taken at Azzano Decimo in the Friulian foreland of northeastern Italy, optically stimulated luminescence (OSL) has been applied to fine grain quartz. The samples meet all the standard performance criteria set to test the reliability of the single-aliquot regenerative-dose (SAR) protocol, and still show increasing dose response at 500 Gy. OSL ages are in good agreement with radiocarbon dating and the pollen interpretation down to 70 ka, and with D_e values of ～140 Gy, but below this point, they display an increasing age underestimation towards the Eemian and beyond. The comparison of D_e values measured using both a SAR and single-aliquot regeneration and added-dose (SARA) protocol, confirmed that both were successfully correcting for sensitivity changes in the quartz during measurement of the burial dose, and this was not the reason for the age underestimation. The quartz OSL dose response curve for all samples is best described by a saturating exponential plus linear (SEPL) function. Although all underestimated ages are derived from D_e values that fall on the high dose linear region of this curve, it is unclear if this is the cause of the underestimation.     

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.     

Variations in luminescence properties of quartz and feldspar from modern fluvial sediments in three rivers

Studies of modern sediments, their sedimentology and depositional processes are important for understanding the behaviour of the luminescence characteristics of quartz and feldspar in fluvial settings. Previous studies have shown large variations in OSL characteristics of quartz from different fluvial systems, while the IRSL and pIRIR signals from K-feldspar have been understudied. We test the effects of fluvial setting on luminescence characteristics by collecting modern (<1 year old) bedload sediments down the courses of three river systems with very different hydrological characteristics, geologic contexts, and catchment lithologies. The single grain (SG) and multi-grain aliquot (MGA) OSL (quartz) and IRSL and pIRIR (K-feldspar) properties of samples were measured and compared to better understand intra- and inter-fluvial system patterns in sensitivity, bleaching, and equivalent dose (D_e) distribution skewness and kurtosis. The quartz OSL and K-feldspar IRSL and pIRIR signal sensitivities increase with downstream transport distance of sediments, confirming previous studies (quartz) and showing that IRSL signals from K-feldspar also increase in response to reworking cycles. Increasing transport distance also results in better bleaching of the OSL signal from quartz samples (MGA and SG) due to more grains being exposed to sunlight. By contrast, the IRSL and pIRIR signals retain significant residuals in all samples, though 5–15% of grains yield zero-dose D_e values and age modelling of SG data yields accurate burial dose estimates. Additionally, the skewness and kurtosis of SG OSL D_e datasets from one river increase with transport distance, with the best bleached samples exhibiting the highest skewness, thereby questioning the applicability of the skewness-value of a D_e dataset as an accurate indicator for partial-bleaching. Our data shows marked variability between (i) different river systems and (ii) the measured minerals, however consistent use of statistical models allows accurate D_e estimation in all contexts. Age modelling of SG data from K-feldspar, thus, provides a valuable tool for future fluvial research in regions where poor OSL characteristics prevent the use of quartz as a dosimeter.