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.     

Changes in natural OSL sensitivity during single aliquot regeneration procedure and their implications for equivalent dose determination

Measurement of low temperature (90°C–120°C) Thermoluminescence (TL) sensitivity of natural quartz samples subjected to pre-heating and optical stimulation indicate that significant sensitivity changes can occur during measurement of the natural Optically Stimulated Luminescence (OSL). During the measurement of natural signal, the luminescence sensitivity of samples can change by 40%. The sensitivity changes both during the initial preheat and the measurement of natural OSL. The currently used version of Single Aliquot Regeneration (SAR) protocol measures and corrects for the sensitivity changes after preheat and readout of natural OSL. However, it does not take into account the changes in sensitivity during the readout of the natural signal. We therefore developed a correction procedure so that both the natural and the regenerated OSL intensities can be measured and plotted with the same sensitivity and suggest that in the absence of such a correction, a considerable fraction of the SAR based ages could have systematic errors. The correction for the sensitivity is based on the use of sensitivity of 110°C TL quartz peak, which is correlated to OSL signal (Murray and Roberts, 1998). The use of 110°C peak provides a reasonable measure of the changes in OSL sensitivity of quartz. A modified Natural Sensitivity Corrected-SAR (NSC-SAR) procedure, that comprises the measurement of, 1) the TL intensity of 110°C peak for a test dose on sample as received (i.e. natural sample) and, 2) the sensitivity of the 110°C peak of the same sample after the preheat and read out of the natural OSL, is proposed. This ratio, termed as Natural Correction Factor (NCF), then provides a way to correct for sensitivity changes. Results on samples from diverse depositional environments indicated that the NSC-SAR consistently (without exception) provided improved distribution in paleodoses i.e. a lower scatter compared to the standard SAR protocol. In addition, the use of this protocol also resolved anomalous cases where the intensity of natural OSL was significantly above the saturation intensity of the regenerated OSL. Implicitly, this study implies a caution on the use of palaeodoses obtained from single grains as such a correction is not possible in the currently used automated single grain OSL measurement systems. The only way now on will be to analyze aliquots with only a grain on them.     

Optically stimulated luminescence (OSL) dating investigations of rock and underlying soil from three case studies

Three rock samples and associated underlying surface (floor) soils of geoarchaeological significance from Greece, Sweden and a modern surface stone-sample from a Danish site were investigated using OSL dating. Thin slice, sub-samples, from drilled core surfaces were prepared. A single-aliquot regenerative-dose (SAR) protocol was used on whole rock slices to estimate the laboratory equivalent dose. Laboratory tests showed that the SAR protocol successfully corrected for sensitivity changes and that a known laboratory dose could be measured accurately.     

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.     

瓷器热释光测定年代研究

本工作从标准的(即线性的)前剂量技术着手,研究了瓷器热释光测定年代的方法。在这个研究中,发现了瓷器的灵敏度对剂量的非线性响应和灵敏度随剂量变化的指数模式。因此,一个用饱和指数拟合的方法被提了出来。实验表明,这是一个测定瓷器年代的成功方法。另外,还对一些与测定年代有关的复杂因素进行了讨论。例如,当少数瓷器的灵敏度与剂量不呈指数关系时,就要改变拟合模式或采用B的平均值方法等。     

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.     

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.     

Detailed protocol for an accurate non-destructive direct dating of tooth enamel fragment using Electron Spin Resonance

In the context of human evolution, fossil remains are too valuable to be destroyed and any alteration should be kept to a minimum. The newly developed protocol on fossil fragments has open the gate for ‘virtually’ non-destructive ESR (Electron Spin Resonance) direct dating of human remains. The method allows the separation of unstable and interfering signals that were responsible for large dose underestimation. While a complete investigation of the ESR signal remains a complex task and requires numerous hours of manipulations, a rapid dose assessment protocol can be achieve without compromising the accuracy nor the integrity of the sample. The new protocol should be used for future dating regardless of the possibility of measuring powder.     

On the intrinsic accuracy and precision of luminescence dating techniques for fired ceramics

Luminescence dating techniques have been used extensively for archaeological and geological samples. Such techniques are based on thermally or optically stimulated signals. This paper presents simulations of several luminescence techniques for equivalent dose (ED) estimation for ceramic materials containing quartz. The simulations are carried out using a recently published comprehensive kinetic model for quartz, consisting of 11 electron and hole traps and centers. The complete sequence of the experimental protocols for several thermoluminescence (TL) and optically stimulated luminescence (OSL) techniques are simulated using the same set of kinetic parameters. The specific simulated protocols are: additive dose TL protocol, predose technique (both additive and multiple activation versions), phototransfer protocol, single aliquot regenerative optically stimulated luminescence (SAR-OSL) protocol, and SAR thermoluminescence protocol (SAR-TL). One hundred random variants of the natural samples were generated by keeping the transition probabilities between energy levels fixed, while allowing simultaneous random variations of the concentrations of the 11 energy levels. The relative intrinsic accuracy and precision of the protocols are simulated by calculating the equivalent dose (ED) within the model, for a given natural burial dose of the sample. The intrinsic accuracy of these techniques is estimated by simulating natural irradiation of the samples with a known burial dose, followed by simulation of the luminescence method used to recover the estimated dose ED. The percent difference between the burial dose and the ED value represents the simulated accuracy of the luminescence technique. The relative intrinsic precision of these techniques is estimated by fitting Gaussian probability functions to the ED values obtained with the 100 model variants. It is found that the various techniques can reproduce natural paleodoses in the range 10 mGy–10 Gy with a typical intrinsic accuracy of +1 to 10%. Techniques based on single aliquot protocols were found in general to be more precise than techniques requiring the use of multiple aliquots. In addition, techniques based on interpolation of experimental data were found to be consistently both more precise and accurate than those based on extrapolation of experimental data.     

Investigating the resetting of OSL signals in rock surfaces

There are many examples of buried rock surfaces whose age is of interest to geologists and archaeologists. Luminescence dating is a potential method which can be applied to dating such surfaces; as part of a research project which aims to develop such an approach, the degree of resetting of OSL signals in grains and slices from five different cobbles/boulders collected from a modern beach is investigated. All the rock surfaces are presumed to have been exposed to daylight for a prolonged period of time (weeks to years). Feldspar was identified as the preferred dosimeter because quartz extracts were insensitive. Dose recovery tests using solar simulator and IR diodes on both K-feldspar grains and solid slices taken from the inner parts of the rocks are discussed. Preheat plateau results using surface grains and slices show that significant thermal transfer in naturally bleached samples can be avoided by keeping preheat temperatures low. Equivalent doses from surface K-feldspar grains were highly scattered and much larger than expected (0.02 Gy to >100 Gy), while solid surface slices gave more reproducible small doses (mean = 0.17±0.02 Gy, n = 32). Neither crushing nor partial bleaching were found to be responsible for the large scattered doses from grains, nor did the inevitable contribution from Na-feldspar to the signal from solid slices explain the improved reproducibility in the slices. By modelling the increase of luminescence signal with distance into the rock surface, attenuation factors were derived for two samples. These indicate that, for instance, bleaching at a depth of 2 mm into these samples occurs at about ∼28% of the rate at the surface. We conclude that it should be possible to derive meaningful burial doses of >1 Gy from such cobbles; younger samples would probably require a correction for incomplete bleaching.     

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.     

AUTO-REGENERATIVE THERMOLUMINESCENCE DATING USING ZIRCON INCLUSIONS

Fired ceramics containing zircon inclusions have been dated by allowing the zircons to regenerate their own thermoluminescence (TL) signal, hence auto-regenerative TL dating. The technique is conceptually straightforward. One first measures the TL accrued since the last heating of the material. The zircon grains are then stored for six months and the TL signal regenerated through self-irradiation is measured. Since the internal dose-rate for zircon is dominated by the internal component the age of the sample is simply given by the ratio of the natural to auto-regenerated signal times the laboratory storage period. The technique, however, requires the measurement of a very small auto-regenerated signal, which introduces a number of experimental and physical complications. The methods for overcoming these problems and successfully dating zircons by auto-regeneration are described.     

Residual doses and sensitivity change of post IR IRSL signals from potassium feldspar under different bleaching conditions

The residual doses and sensitivity change for potassium-rich feldspar (K-feldspar) have been studied using the post-infrared infrared stimulated luminescence (pIRIR) and multi-elevated-temperature post-IR IRSL (MET-pIRIR) protocols. Laboratory simulated poorly-bleached and well-bleached samples were those K-feldspar grains bleached using a solar simulator for 10 minutes and 8 hours, respectively. The residual doses rise with stimulation temperature and time. The poorly-bleached sample has larger residual doses than the well-bleached sample, especially at high stimulation temperatures. The high-temperature pIRIR signals contain a large amount of hard-to-bleach signals. A decrease of luminescence sensitivity was observed after conducting a high-temperature-treatment in the measurement cycles. The sensitivity decreases significantly between the first and the second cycle. The extent of decrease in sensitivity shows a clear temperature trend. The higher the stimulation temperature of pIRIR signals is, the larger the sensitivity decreases. This decrease is more severe for the poorly-bleached sample than for the well-bleached sample, and could possibly lead to problems in sensitivity correction.     

Historical mortars dating from OSL signals of fine grain fraction enriched in quartz

In the last years the mortar dating through Optically Stimulated Luminescence (OSL) techniques has become a viable support for chronological estimations (date of construction or restoration episodes) of historical buildings. However, the dating of mortar has still open issues mainly regarding the assessment of the bleaching degree of quartz, the analysis of the OSL processes for this type of samples and the need to do appropriate tests for the most correct evaluation of the equivalent dose. This paper discusses the results obtained by OSL dating (blue diode stimulation) on the polymineral fine grain phase, enriched in quartz, extracted from lime mortar samples collected from different sites. Thermal transfer effects, through the behaviour of Equivalent Dose (ED) and recovery tests, degree and time of bleaching were studied. For each mortar sample the adjacent brick was collected; in some cases, sampling of the bricks bracketing a mortar layer was a possibility, thus obtaining a direct comparison with the standard thermoluminescence (TL) dating on the bricks. The results obtained show, for this set of samples, the possibility of dating the mortars through the use of the fine grain fraction provided of a suitable chemical-physical preparation procedure and the verification of the bleaching conditions.     

OSL and TL dating of the Middle Stone Age sequence at Diepkloof Rock Shelter (South Africa): a clarification

Diepkloof Rock Shelter offers an exceptional opportunity to study the onset and evolution of both Still Bay (SB) and Howiesons Poort (HP) techno-complexes. However, previous age estimates based on luminescence dating of burnt quartzites (Tribolo et al., 2009) and of sediments (Jacobs et al., 2008) were not in agreement. Here, we present new luminescence ages for 17 rock samples (equivalent dose estimated with a SAR-ITL protocol instead of classical MAAD-TL) as well as for 5 sediment samples (equivalent dose estimated with SAR-single grain OSL protocol) and an update of the 22 previous age estimates for burnt lithics (modified calibration and beta dose estimates). While a good agreement between the rock and sediment ages is obtained, these estimates are still significantly older than those reported by Jacobs et al. (2008). After our own analyses of the sediment from Diepkloof, it is suspected that these authors did not correctly chose the parameters for the equivalent dose determination, leading to an underestimate of the equivalent doses, and thus of the 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 PRE-DOSE TECHNIQUE: A NEW THERMO-LUMINESCENT DATING METHOD

A thermoluminescent (TL) glow-curve peak occurs around 110°C for the mineral quartz. Its sensitivity may be changed by application of a radiation dose (termed the pre-dose) followed by a heating of the quartz to 500°C: heating alone causes no sensitivity change. The enhancement observed (measured relative to the sensitivity of the peak prior to heating) is a measure of the magnitude of the pre-dose. For quartz extracted from pottery the sensitivity enhancement induced by laboratory heating records a natural pre-dose, i.e. the accumulated dose experienced during archaeological burial. The latter quantity is used in TL age-determination and a test programme is reported on the application of the pre-dose dating method to sites covering the Roman era in Britain forward to modern times.     

OPTICAL DATING OF ANTHROPOGENIC SEDIMENTS AT THE ARCHAEOLOGICAL SITE OF HERRENBRUNNENBUCKEL,BRETTEN-BAUERBACH (GERMANY)*

Optical dating was applied to natural and anthropogenic silts at an Iron Age settlement in southern Germany. The natural sediments were dated accurately and allowed study of the human impact on the landscape. The studied anthropogenic sediments were infills of cellars and ditches. Again, deposits derived from soil erosion proved to be datable using infrared-optically stimulated luminescence. However, optical dating of fine grained sediments was at its limits when sediments consisted of a mixture of bleached and unbleached grains. This is shown on sediments of known age originating from cellar infills. Improvements were obtained when using the 560 nm emission and a partial bleach approach. Experimental evidence shows that the D_E versus shine-time plot discloses insufficient bleaching only in cases in which all grains are insufficiently bleached to the same degree.     

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.     

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.