Construction of a quartz OSL standardised growth curve (SGC) for aeolian samples from the Horqin dunefield in northeastern China

It has been suggested that the standardised growth curve (SGC) method can be used to de-terminate D_e accurately and reduce the measurement time. However, different opinions regarding the applicability of the SGC method exist. In this paper, we report the construction of quartz OSL SGC for 35 aeolian samples from different parts of the Horqin dunefield in northeastern China, and then test their applicability for D_e determination. Our results suggest that: 1) up to a regeneration dose of 80 Gy, the SGC of the Horqin dunefield can be fitted using the exponential plus linear equation, with the r² value of 0.97, and all the regeneration dose points closely stick to the fitting line, implying that all samples share a very similar dose-response curve; 2) for samples with Des ranging from 1 to 50 Gy, the ratios of SAR D_e to SGC D_e fall within the range of 0.9–1.1, and the average ratio of SAR D_e to SGC D_e is 1.01±0.01, close to unity. Therefore, the construction of SGC is correct, and the SGC is an effective procedure for accurate D_e determination for samples from the study area.     

Examining quartz OSL age underestimation for loess samples from Luochuan in the Chinese Loess Plateau

When using quartz OSL to date loess samples from the Chinese Loess Plateau, it has been reported that the agreement between OSL ages and the independent ages is limited to the samples younger than ～70 ka with a corresponding D_e of ～230 Gy, and a sample with an expected age of 780 ka was dated to 107 ka, corresponding to 403 Gy. The growth curves of these samples do not saturate at doses of 700 Gy, and a linear growth part was observed for doses higher than 200 Gy. However, the maximum measured age of ～100 ka imply that the D_e determined using this linear part of a growth curve could be problematic, or that the quartz OSL signal is not as stable as previously thought and has a barrier age of ～100 ka. In the current study, we examine the reasons for the age underestimation. We examined the shape of growth curves, anomalous fading, thermal stability, etc. The results show that, for the loess samples examined, quartz OSL does not fade anomalously, and the barrier age of ～100 ka is due to the fact that the OSL signals are less thermally stable, the lifetime of 0.311 Ma at 20°C obtained is much smaller than those for quartz samples from other regions such as Australia (～100 Ma).     

Geoarchaeological studies on Roman time harbour sediments in Cologne — comparison of different OSL dating techniques

Due to the construction of a new North-South subway in Cologne, Roman time harbour sediments were exposed and were sampled for luminescence dating. A very good independent age control was given by the precise knowledge of the chronology of Roman activity and by radiocarbon ages of charcoal samples. Hence, different methodological approaches within luminescence dating were applied for Holocene heterogeneously bleached fluvial samples and were compared to the known ages. For one sample, optically stimulated luminescence (OSL) dating was applied to coarse-grained quartz using a single aliquot regenerative-dose (SAR) protocol. After D_e-measurements, different statistical approaches were tested (i.e. arithmetic mean, median, minimum age model, finite mixture model, leading edge method and the Fuchs and Lang approach). It is demonstrated that the Fuchs and Lang approach along with the leading edge method yielded the best matching OSL ages with respect to the known ages.     

Comparison of three K-feldspar luminescence dating methods for Holocene samples

The luminescence dating of the K-feldspar fraction is an alternative way for samples that cannot yield reasonable equivalent dose (D_e) from quartz fraction with very weak luminescence signal. For testing the reliability of the infrared stimulated luminescence (IRSL) dating of K-feldspar, luminescence dating was applied to quartz and K-feldspar fractions respectively for several Holocene samples in this study. K-feldspar apparent ages using routine single aliquot regenerative-dose (SAR) protocol, K-feldspar ages using g value correction method and ages from isochron dating method were compared with quartz ages. It is found that the g value correction method cannot give reliable ages due to the large errors induced during measurements. The isochron dating method is effective to the sample with problematically external dose rate. However, isochron dating may introduce a relatively greater error during grain sizes — D_e curve fitting, therefore this method could obtain low-resolution ages for Holocene samples. Even K-feldspar apparent age from routine SAR protocol is relatively younger by about 10% than the quartz age, it still could establish reasonable chronological framework for Holocene samples.     

Investigations on the degree of bleaching of quartz OSL signals using modern aeolian dust from western Loess Plateau, China

Optically Stimulated Luminescence signal of quartz extracted from modern aeolian dust with known maximum age (about decades) was analyzed in terms of degree of bleaching. The results of dose recovery tests show that the modified double single-aliquot regenerative-dose protocol with the early background subtraction is robust for dating these modern dusts using small aliquots. Bleaching of these dusts is discussed based on the distribution of De values in histograms, scatter plots of D_e versus sensitivity corrected natural OSL signal and comparison between measured D_e and expected D_e. The results indicate that most dusts were completely bleached but some dusts were not completely bleached. For those incompletely bleached dusts in Lanzhou area, the maximum OSL age overestimation is up to ～1 ka, which might be caused by fast deposition accompanied by heavy sand/dust storms. The research suggests that cautions should be given to OSL ages younger than 1 ka in the western China close to deserts.     

Optically stimulated luminescence dating of young fluvial deposits of the Middle Elbe River Flood Plains using different age models

In the last few decades optically stimulated luminescence (OSL) dating has become an important tool in geochronological studies. The great advantage of the method, i.e. dating the depositional age of sediments directly, can be impaired by incomplete bleaching of grains. This can result in a scattered distribution of equivalent doses (D_E), leading to incorrect estimation of the depositional age. Thoroughly tested protocols as well as good data analysis with adequate statistical methods are important to overcome this problem. In this study, samples from young fluvial sand and flood plain deposits from the Elbe River in northern Germany were investigated to compare its depositional ages from different age models with well-known historical dates. Coarse grain quartz (100–200 μm and 150–250 μm) and polymineral fine grains (4–11 μm) were dated using the single aliquot regenerative (SAR) dose protocol. The paleodose (D_P) was calculated from the DE data set using different approaches. Results were compared with the development of the Elbe River, which is well-documented by historical records and maps covering the last 1,000 years. Depending on the statistical approach it can be demonstrated that depositional ages significantly differ from the most likely depositional age. For the investigated coarse grain quartz samples all ages calculated from the MAM-3_UL, including their uncertainties, are within the historical documented age. Results of the polymineral fine grain samples are overestimating the historically documented depositional age, indicating undetectable incomplete bleaching. This study shows the importance of using an adequate statistical approach to calculate reliable OSL ages from fluvial sediments.     

An improved OSL chronology for the Still Bay layers at Blombos Cave,South Africa: further tests of single-grain dating procedures and a re-evaluation of the timing of the Still Bay industry across southern Africa

This paper presents a series of new single-grain optically stimulated luminescence (OSL) ages for the Still Bay at Blombos Cave, South Africa, and compares them to previously published OSL, thermoluminescence (TL) and electron-spin resonance (ESR) ages for this site. Details are provided about the measurement and analytical procedures, including a discussion of the characteristics of the OSL signals of individual quartz grains. This forms the basis for further investigations into the sensitivity of the equivalent dose (D_e) estimates to a range of different analytical approaches, including changes in the size of the test dose, the choice of signal integration interval, the subtraction of an appropriate background, and isolation of the most light-sensitive (‘fast’) component of quartz OSL. We also report the results of an inter-operator test of D_e determination using seven new samples from Blombos Cave, and demonstrate the reproducibility of results obtained for two samples that had been dated previously at another laboratory and were measured and analysed again in this study. Together, these tests validate the robustness of the Blombos Cave single-grain OSL age estimates to a variety of alternative OSL dating procedures. We have incorporated, for the first time, these ages for Blombos Cave into a data set of all single-grain OSL ages for Still Bay and Howieson's Poort sites across southern Africa, and have used a statistical model to re-evaluate the timing and duration of the Still Bay industry. We calculate the most plausible start and end dates of the Still Bay as 72.2 ka and 71.3 ka, respectively – amounting to a duration of 0.9 ka – and estimate (with conventional 95% confidence) that this industry began no earlier than 75.5 ka, ended no later than 67.8 ka and lasted no longer than 6.6 ka.     

Performance of different luminescence approaches for the dating of known-age glaciofluvial deposits from northern Switzerland

Luminescence properties of two samples taken from sand lenses in proglacial outwash de-posits of a piedmont glacier that reached the Swiss midlands during the Last Glacial Maximum are investigated in detail. Deconvolution of CW-OSL decay curves shows that the fast component dominates the OSL signal of quartz. The chemistry of single feldspar grains, in particular the K content in different grains, is determined using wavelength dispersive spectrometry (electron microprobe), revealing an average 12.9 wt.% K of the grains contributing to the IRSL signal. D _e distributions are investigated in order to gain insights into partial bleaching, and agreement is found for quartz OSL and feldspar IR₅₀ and pIRIR₂₂₅ ages for small aliquots and single grains when applying the Minimum Age Model. These ages are also consistent with independent age control. For one sample, ages determined using the Central Age Model result in highly overestimated ages for both feldspar and quartz.     

OSL dating using quartz fine grains extracted from loess in Upper Palaeolithic sites of Nihewan Basin, northern China

Although radiocarbon (¹⁴C) dating, uranium-series dating, and optically stimulated luminescence (OSL) dating have been conducted for Upper Palaeolithic sites in the Nihewan Basin, northern China, there is room for constructing a detailed chronological framework. In this study, loess sediments collected from two Upper Palaeolithic sites, Youfang site and Hutouliang site, were dated using the single-aliquot regenerative-dose (SAR) OSL protocol. OSL measurements for palaeodoses estimation used fine-grained quartz samples extracted from loess. OSL dating results were obtained as 10–17 ka. These OSL ages were consistent with the related stratigraphy of Palaeolithic sites, archaeological evidence and independent ¹⁴C ages.     

Expectations of scatter in equivalent-dose distributions when using multi-grain aliquots for OSL dating

In the OSL dating of sediment, the scatter in equivalent dose (D _e) between grains is almost always larger than would be expected due to counting statistics alone. Some scatter may be caused by insufficient (partial) bleaching of some of the grains prior to deposition. In order to date partially bleached sediment, it is essential to estimate the amount of scatter caused by other processes (e.g. grain-to-grain variability in the natural dose rate). Measurements of such scatter are performed at the single-grain level; by contrast, most OSL dating is performed on multi-grain subsamples, for which grain-to-grain scatter is reduced through averaging.     

The D e (T,t) plot: A straightforward self-diagnose tool for post-IR IRSL dating procedures

This study presents a new self-diagnose method for the recently developed post-IR infrared stimulated luminescence (pIRIR) dating protocols. This criterion studies the dependence of equivalent dose (D _e) on measurement-temperature (T) and time (t), by applying the D _e (t) analysis to the IRLS and pIRIR signals measured under different temperatures, and combines these D _e (t) plots into one, so-called the D _e (T, t) plot. The pattern of the D _e (T, t) plot is shown to be affected by anomalous fading, partial bleaching and non-bleachable signal. A D _e plateau can be achieved in the D _e (T, t) plot only when the effects of these factors are insignificant. Therefore, this plot can be used as a self-diagnose tool for the validity of pIRIR results. The D _e (T, t) analysis has been applied to four recently developed pIRIR protocols, using aeolian samples with different ages. The results show that this self-diagnose tool can be applied to different pIRIR protocols for validating the pIRIR dating results and evaluating the pIRIR measurement conditions.     

Luminescence dating of volcanogenic outburst flood sediments from Aso volcano and tephric loess deposits, southwest Japan

Luminescence dating has been applied to volcanogenic outburst flood sediments (Takuma gravel bed) from Aso volcano, Japan, and tephric loess deposits overlying the gravel bed. The poly-mineral fine grains (4–11 μm) from loess deposits were measured with pulsed optically stimulated luminescence (pulsed OSL) and post-IR infrared stimulated luminescence (pIRIR) methods, whereas the Takuma gravel bed containing no quartz, was measured with IRSL and pIRIR methods using sand sized (150–200 μm) plagioclase. The loess deposits date back at least to ～50 ka by consistent IRSL, pIRIR and pulsed OSL ages from the lowermost part of the loess deposits from one section. The ages obtained from the bottom part of the other loess section are not consistent each other. However, we consider that the pIRIR age (72±6 ka) which showed negligible anomalous fading is most reliable, and regard as a preliminary minimum age of the Takuma gravel bed. The equivalent doses (D_e) for the plagioclase from the Takuma gravel bed have a narrow distribution and the weighted mean of the three samples yield an age of 89±3 ka. This age is in agreement with the last caldera-forming eruption of Aso volcano (～87 ka) and it is likely that the pIRIR signal has not been bleached before the deposition. IRSL dating without applying pIRIR using small aliquots was also conducted, however, the IRSL signal shows no clear evidence of an additional bleaching during the event of outburst flood from the caldera lake.     

Review and assessment of the potential of post-IR IRSL dating methods to circumvent the problem of anomalous fading in feldspar luminescence

Quartz has been the main mineral used for optically stimulated luminescence (OSL) dating of sediments over the last decade. The quartz OSL signal, however, has been shown to saturate at relatively low doses of ～200–400 Gy, making it difficult to be used for dating beyond about 200 thou-sand years (ka), unless the environmental dose rate is low. The infrared stimulated luminescence (IRSL) from feldspars has been shown to continue to grow to higher dose levels than quartz OSL. The application of IRSL dating of feldspars, however, has long been hampered by the anomalous fading effect. Recent progress in understanding anomalous fading of the infrared stimulated luminescence (IRSL) signals in potassium-feldspar has led to the development of post-IR IRSL (pIRIR) protocols and also a multiple elevated temperature (MET) stimulation (MET-pIRIR) protocol. These procedures have raised the prospect of isolating a non-fading IRSL component for dating Quaternary deposits containing feldspars. In this study, we review the recent progress made on (1) overcoming anomalous fading of feldspar, and (2) the development of pIRIR dating techniques for feldspar. The potential and problems associated with these methods are discussed.     

IRSL and post-IR IRSL residual doses recorded in modern dust samples from the Chinese Loess Plateau

Using a set of modern/young (0 to about 200 years old) dust samples collected from the Chinese Loess Plateau the bleachability of IRSL measured at 50°C (IR₅₀) and post-IR₅₀ elevated temperature IRSL (measured at 225°C and at 290°C) is investigated by measuring the apparent (residual) doses recorded by these signals. Doses recorded by quartz OSL are used as a reference. Allowing for differences in dose rates it seems that both IRSL and post-IR IRSL signals yield residual doses that are significantly larger than the doses measured in quartz. These residual doses can be largely explained by thermal transfer caused by preheating. Nevertheless, we advise against the use of a low temperature preheat (<200°C) with IR₅₀ to date loess samples because, as has been reported before, the signal appears to be thermally unstable. In general, we conclude that it may not be advisable to apply post-IR IRSL dating to Chinese loess samples where residuals of up to ∼20 Gy are a significant fraction of the total dose. However, these residuals quickly become unimportant when dating older samples, and this is the age range in which post-IR IRSL dating is likely to be most useful.     

Optically stimulated luminescence dating of heated materials using single-aliquot regenerative-dose procedure: a feasibility study using archaeological artefacts from India

Optically stimulated luminescence (OSL) dating of heated/fired materials of archaeological importance from various parts of India was attempted. A single-aliquot regenerative-dose (SAR) procedure was used for palaeodose determination in the quartz grains extracted from the heated materials using the luminescence produced by blue light stimulation. In most pottery samples, the palaeodose obtained using SAR-OSL is ∼6% lower than the palaeodose measured using thermoluminescence (TL) method. Broadly, there is good agreement between the SAR-OSL and TL ages of the artefacts and their archaeologically expected ages. The results suggest that routine dating of heated/fired materials using the SAR-OSL procedure is more practicable, especially when the TL sensitivity of the quartz grains is poor and availability of datable material is limited.     

OSL and TL characteristics of fine grain quartz from Mongolian prehistoric pottery used for dating

The OSL, post-IR OSL and pulsed post-IR OSL applied to polymineral grains and calculated by fitting to the data the contributions from fast, medium and slow components revealed that the polymineral samples under study are dominated by the medium component. An increase in D _e ’s with increasing integration intervals was observed, which is considered as an indication of increasing medium and decayed fast component; and the equivalent doses obtained using different components or minerals reflect also the shape of the dose distributions. The identified fast component in polymineral sample has photoionization cross section of 1.2±0.02 × 10^?17 cm². The present study shows the usefulness of the application of different luminescence techniques combined with fitting procedures as a check which should be adopted in dating protocols. Based on luminescence ages obtained on poly-mineral grains from prehistoric pottery samples from the Boroo settlement, Mongolia, which are in agreement with independent age control by ¹⁴C on charcoal material, it is argued that the manufacturing of Xiongnu — pottery at this site lasted until ca. 130±75 AD.     

Luminescence characteristics and dose distributions for quartz and feldspar grains from Mumba rockshelter,Tanzania

Mumba rockshelter is a key archaeological site for the Middle and Later Stone Age occupation of East Africa, but its chronology has remained unresolved. We report the results of a dating study, focussing on the characterisation of the optically stimulated luminescence (OSL) and infrared stimulated luminescence (IRSL) properties of quartz- and potassium-rich feldspar grains. Quartz has previously proven troublesome for dating in East Africa. We identified five general types of quartz grain behaviour, based on the shapes of their OSL decay and dose–response curves. Dose recovery experiments and measurement of the natural samples revealed particular problems with quartz grains that had hyperbolic dose–response curves, low characteristic saturation doses and anomalously large changes in sensitivity between regenerative-dose cycles. The use of pulsed irradiation during measurement and standard and additional quality-assurance criteria during data analysis reduced the number of grains that suffered from these problems. We applied these procedures to individual grains of quartz from eight samples and, using appropriate statistical models, identified post-depositional mixing in three samples. The remaining samples had scattered equivalent-dose distributions typical of quartz grains that had received variable beta dose rates during burial. Stratigraphically consistent OSL ages were obtained for all but the deepest sample. Feldspar ages were estimated for the latter sample and three other samples, using the elevated temperature IRSL signal that exhibited low rates of anomalous fading. Fading-corrected feldspar ages for the latter three samples are consistent with their single-grain quartz ages, but single-grain dating is needed to address problems of post-depositional mixing.     

Comparing different post-IR IRSL approaches for the dating of Holocene coastal foredunes from Ruhnu Island,Estonia

Different post-IR Infrared Stimulated Luminescence (IRSL) approaches are applied to sediments from a Holocene coastal foredune sequence on Ruhnu Island in the eastern Baltic Sea. The comparison of D _e-values and ages determined by the different approaches is complimented by fading and bleaching experiments. The fading experiments imply strong fading of IRSL (50°C) signals and no fading of any of the post-IR IRSL signals, but this is not confirmed by the determined D _e-values. In fact, post-IR IRSL (150°C) D _e-values agree within errors with those calculated for IRSL (50°C). From the bleaching experiments it is inferred that the higher values observed for post-IR IRSL at more elevated stimulation temperatures (225°C/290°C) are likely related to either thermal transfer and/or slow-to-bleach components within the signal. For the dating of the Holocene foredune sequence of Ruhnu Island, the post-IR IRSL (150°C) approach is preferred and these agree with the limited independent age control available from radiocarbon dating. Accordingly, the sequence formed between ca. 7.0 ka and 2.5 ka ago.     

Equivalent dose distributions from single grains of quartz at Sibudu,South Africa: context,causes and consequences for optical dating of archaeological deposits

Optical ages for 14 sediment samples collected from the post-Howiesons Poort, late Middle Stone Age (MSA) and final MSA deposits at Sibudu, KwaZulu-Natal, South Africa were reported in a companion paper (Jacobs, Z., Wintle, A.G., Duller, G.A.T., Roberts, R.G., Wadley, L. New ages for the post-Howiesons Poort, late and final Middle Stone Age at Sibudu, South Africa. Journal of Archaeological Science, 2008). These ages were based on equivalent dose (D_e) distributions that were overdispersed. In this paper, we investigate factors both internal and external to the grains that may contribute to such higher than expected overdispersion in single grain D_e values. Intrinsic factors accounted for some, but not all, of the observed scatter, and application of a set of rejection criteria filtered grains for which erroneous D_e values would otherwise be calculated. We investigated sediment mixing and differences in the beta dose received by individual grains in their burial environment as two likely reasons for the observed overdispersion. The scatter in D_e distributions for all the samples is best explained by grains that were deposited at the same time and which were well bleached, but that subsequently received a range of beta doses. A procedure is presented for adjusting the measured beta dose rate, and its associated error. We show that using a combination of single grain OSL measurements of D_e, the finite mixture model and adjustment of the beta dose rate, result in stratigraphically consistent ages. These ages are more consistent than the ages obtained from multiple grain aliquot D_e values and the average dose rates for each sample; the multiple grain ages are about 10% older, partly because of the variable dose rate and partly because these aliquots contained grains with undesirable OSL characteristics.     

Single-grain OSL dating at La Grotte des Contrebandiers (‘Smugglers’ Cave’), Morocco: improved age constraints for the Middle Paleolithic levels

Optically stimulated luminescence (OSL) measurements of individual quartz grains are reported for Middle Paleolithic (MP) or Middle Stone Age (MSA) deposits in La Grotte des Contrebandiers, Morocco. Single-grain measurements enable rejection of grains that may lead to under- or over-estimation of age due to malign luminescence properties or remobilisation of grains after burial. We identified the former using a range of experimental procedures and objective rejection criteria. Three post-depositional factors influenced the distribution pattern of equivalent dose (D_e) values for the remaining single grains: the disintegration of roof spall liberating unbleached, older grains into otherwise well-bleached sediments; the intrusion of a small number of younger grains from the overlying Upper Paleolithic deposits; and small-scale differences in the beta dose received by individual grains. Roof spall contamination was a significant problem, so we characterised the OSL signals and obtained D_e values for the calcareous sandstone in which the cave is formed, which allowed bedrock-derived grains in the MP/MSA deposits to be identified and rejected prior to age determination. We collected 31 samples from the MP/MSA deposits, and were able to calculate ages for 30 of them. These ages suggest that MP/MSA occupation of Contrebandiers was restricted to the interval between about 120 and 90 ka ago (Marine Isotope Stages 5d to 5b). Weighted mean OSL ages were obtained for samples associated with archaeologically sterile deposits at the base of the excavations (126 ± 9 ka), followed by two phases of the Moroccan Mousterian (122 ± 5 and 115 ± 3 ka), interspersed with archaeologically sterile deposits (112 ± 4 ka). The base and top of the Aterian were dated to 107 ± 4 and 96 ± 4 ka, respectively. Based on the grand weighted mean ages of 116 ± 3 and 103 ± 3 ka for the Moroccan Mousterian and Aterian at Contrebandiers, we suggest that these two industries may be separated by an occupation hiatus of up to 13 ± 3 ka at this site. Our single-grain OSL chronology confirms previous age estimates obtained for Contrebandiers and other sites in the vicinity, but are generally more precise and stratigraphically more coherent, due to the inherent advantages of measuring individual quartz grains and rejecting contaminant and other unsuitable grains before age determination.