Testing the standardized growth curve (SGC) to OSL dating coastal sediments from the south Bohai Sea, China

It has been suggested that the standardized growth curve (SGC) method can be used to accurately determinate equivalent dose (D_e) and reduce measurement time. However, different opinions regarding the applicability of the SGC method exist. In this paper, we evaluated quartz OSL SGCs of marine and coastal sediments of different grain sizes and different cores in the south Bohai Sea in China, and tested their applicability to the determination of D_e values. Our results suggested as follows: (1) The SGC method is applicable to both multiple- and single-aliquot regenerative-dose (MAR and SAR) protocols of OSL dating and efficiently provides reliable estimates of D_e. (2) Finesand quartz of different palaeodoses showed highly similar dose-response curves and an SGC was developed, but old samples using the SGC method have large uncertainties. (3) For coarse-silt quartz, two different types of dose-response curves were recorded: low-dose (≤60Gy) and high-dose (≥100Gy). The growth curves of low-dose quartz were similar to each other, facilitating the use of SGC in D_e estimations, but errors tended to be larger than those obtained in the SAR method. For high-dose (100–300Gy) quartz, the SGC was also found to be reliable, but there was large uncertainty in D_e (>300Gy) estimation. We suggest that SGC could be employed for the dating of marine and coastal sediments dating using either MAR or SAR OSL protocol and either fine-silt, coarse-silt or fine-sand quartz.     

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.     

Constraints on the precision of SAR in equivalent dose estimations close to saturation in quartz

Difficulties in evaluating accurate equivalent doses for Late Quaternary sediments from the south coasts of Greece arose in the course of SAR measurements. Large scatter among apparent equivalent doses perplexed the evaluation of accurate mean estimates in circumstances where very large doses were involved. Besides, dose recovery experiments revealed that when intersection of the natural signal occurs onto the saturating segment of the growth curve, a distinct relationship between D_e and growth curve shape occurs. At very low slope angles, SAR tends to overestimate the recovered dose. The mechanism which controls the spread in equivalent dose estimation is investigated.     

Roman traces in Germania magna: New thermoluminescence and pIRIR290 data from a lime kiln at Bergisch Gladbach,Germany

The applicability of a post‐infrared infrared stimulated luminescence (pIRIR₂₉₀) protocol and two different thermoluminescence (TL) protocols—a single aliquot regeneration (SAR) and a multiple aliquot additive dose (MAAD)—was tested on six polymineral fine‐grain (4–11 μm) samples extracted from the wall remains of a Roman lime kiln and a Roman roof tile. These remains had been excavated close to Bergisch Gladbach, which was at that time part of Germania magna. For the pIRIR₂₉₀ measurements, no dependence of D_e on first‐stimulation temperature was detectable, and the standard first stimulation temperature at 50°C was adopted. Fading tests and dose‐recovery tests were made for all samples. Background subtracted glow curves were recorded up to 480°C for TL after a preheat of 220°C for 120 s. A‐values were determined for all TL and pIRIR measurements. The results for all three protocols were fairly consistent, and TL and pIRIR₂₉₀ protocols are shown to be suitable to estimate reliable equivalent doses for the fired kiln walls. The resulting ages are in agreement with the expected time range—Roman Iron Age—and with independent age control provided by radiocarbon ages of animal bones and charcoal from the firing chamber.     

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).     

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.     

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.     

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.     

Performance tests using the Lexsyg luminescence reader

This study presents test measurements on a Lexsyg luminescence reader, acquired by the Giessen luminescence group. The reader is of the type Standard, hence designed for routine determination of palaeodoses using quartz or K-feldspars. The tests include measurements of the stimulation powers, preheat temperatures, OSL- and TL-curves, as well as dose recovery tests and calibration measurements using highly sensitised calibration quartz. A comparison of D _e values determined using a Lexsyg reader with single grain D _e-values, which have been previously obtained on a Risø reader, is also presented. The results imply that the Lexsyg reader is a highly reliable measurement device with high reproducibility, yielding instrumental uncertainties of around 0.3%.     

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.     

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.     

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 dating studies of Ye?ilova Hoyuk

Ceramic findings collected from Ye?ilova Hoyuk located in Izmir were dated using the thermoluminescence dating technique. The area is of significant archaeological importance since it is the first prehistoric settlement in Izmir. Recent archeological observations suggest that human occupation of the region took place about 8500 years ago comparing to previously determined dates of 5000 years. Three samples collected from the same archaeological layer (Neolithic period) in Ye?ilova Hoyuk were dated using the thermoluminescence method. Archaeological doses (AD) were obtained by single aliquot regenerative dose method (SAR) for thermoluminescence (TL) using coarse grain quartz minerals extracted from samples. Thick and thin Al₂O₃:C thermoluminescence dosimeters (TLD) were used to determine the annual dose rate. The archaeological doses were found to vary from 25.91±0.78 to 26.82±0.68 Gy, and the annual doses were found to be between 3.34±0.24 and 3.47±0.24 mGy/a. The ages obtained for the samples were determined to be 6000±830 BC, 5740±670 BC and 5460±740 years for samples ND1, ND2 and ND3, respectively, which supports the prediction of archeologist that the sampling layer dates from the Neolithic period.     

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.     

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.     

A NEW THERMOLUMINESCENCE DATING TECHNIQUE FOR HEATED FLINT*

A new thermoluminescence (TL) technique for determining the age of heated flint artefacts from archaeological sites is presented. It is a variant of the SAR protocol, which is usually used for OSL dating of sediment, but it is not based on a presumed model for fitting the dose–response curve. Dose recovery tests as well as comparisons with standard protocols show the accuracy of the new technique. It is found that the sensitivity of the thermoluminescence (TL) signal of flint in the orange–red waveband does not show severe changes due to the heating process while measuring the TL. This allows the application of a short SAR procedure, which requires only two dose points. The technique does not require as much instrument time as other SAR techniques, and thus is advantageous for dating very old samples. The major advantage of this new technique is the small amount of sample material required, which allows the dating of samples that are too small for standard TL dating techniques.     

Br/Cl signature of hydrothermal fluids: liquid–vapour fractionation of bromine revisited

Br/Cl ratios of hydrothermal fluids are widely used as geochemical tracers in marine hydrothermal systems to prove fluid phase separation processes. However, previous results of the liquid–vapour fractionation of bromine are ambiguous. Here we report new experimental results of the liquid–vapour fractionation of bromine in the system H₂O–NaCl–NaBr at 380–450°C and 22.9–41.7 MPa. Our data indicate that bromine is generally more enriched than chlorine in the liquid phase. Calculated exchange coefficients K_D(Br‐Cl)^{liquid‐vapour} for the reaction Br^vapour + Cl^liquid = Br^liquid + Cl^vapour are between 0.94 ± 0.08 and 1.66 ± 0.14 within the investigated P–T range. They correlate positively with D_Cl^{liquid‐vapour} and suggest increasing bromine–chlorine fractionation with increasing opening of the liquid–vapour solvus, i.e. increasing distance to the critical curve in the H₂O–NaCl system. An empirical fit of the form K_D(Br‐Cl)^{liquid‐vapour} = a*ln[b*(D_Cl^{liquid‐vapour}?1) + e^1/a] yields a = 0.349 and b = 1.697. Based on this empirical fit and the well‐constrained phase relations in the H₂O–NaCl system we calculated the effect of fluid phase separation on the Br/Cl signature of a hydrothermal fluid with initial seawater composition for closed and open adiabatic ascents along the 4.5 and 4.8 J g^?1 K^?1 isentropes. The calculations indicate that fluid phase separation can significantly alter the Br/Cl ratio in hydrothermal fluids. The predicted Br/Cl evolutions are in accord with the Br/Cl signatures in low‐salinity vent fluids from the 9 to 10°N East Pacific Rise.     

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.     

Investigation of lime mortars and plasters from archaeological excavations in Hippos (Israel) using Electron Paramagnetic Resonance

This study presents the preliminary results of investigation of the lime mortars and plasters from archaeological excavations in Hippos (Israel), using Electron Paramagnetic Resonance (EPR) spectroscopy. The research was conducted in order to characterize the building material and its reaction to ionizing radiation. The ancient settlement Hippos, situated on the east shore of the Sea of Galilee, functioned from the 3^rd cent. BC until it was destroyed by the earthquake in 749 AD. Lime mortars and plasters show carbonate and locally gypsum character of binder and different kind of aggregate. Samples were γ-irradiated and measured using X-band EPR spectrometer. Computer Resolution Enhancement Method was applied to the complex spectra. Some of the γ-induced EPR signals were attributed to CO₂ ^? and CO₃ ^3? paramagnetic centres. Exponential growth of the dose response curve above 1 kGy and saturation for doses above 20 kGy was observed. For doses lower than 1 kGy the dose response curve has a linear character. The presence of γ-sensitive carbonate paramagnetic centres could indicate that, after further studies, well-chosen samples of mortars and plasters might be suitable for EPR dating, assuming the centres have been sufficiently bleached during the manufacturing process.     

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.