An attempt to estimate firing temperature using OSL pre-dose sensitization of quartz

The estimation of firing temperature of ceramics using methods based on pre-dose sensitization of the 110°C TL peak of quartz have yielded incoherent results. Recently the fast component of the CW-OSL of quartz has been observed to have pre-dose characteristics similar to that of the 110°C TL peak. The motivation for this study has been to look into the feasibility of this signal, the OSL counter part of pre-dosed TL emission, for the firing temperature identification. The variation in the sensitization ratio of the TL and OSL emissions with different heating temperatures was also utilized to unveil the firing temperature mark of the specimen.     

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.     

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.     

On the applicability of post-IR IRSL dating to Japanese loess

Recent work on infrared stimulated luminescence (IRSL) dating has focussed on finding and testing signals which show less or negligible fading. IRSL signals measured at elevated temperature following IR stimulation at 50°C (post-IR IRSL) have been shown to be much more stable than the low temperature IRSL signal and seem to have considerable potential for dating. For Early Pleistocene samples of both European and Chinese loess natural post-IR IRSL signals lying in the saturation region of the laboratory dose response curve have been observed; this suggests that there is no significant fading in nature. As a contribution to the further testing of post-IR IRSL dating, we have used 18 samples from two Japanese loess profiles for which quartz OSL and tephra ages up to 600 ka provide age control. After a preheat of 320°C (60 s), the polymineral fine grains (4–11 μm) were bleached with IR at 50°C (200 s) and the IRSL was subsequently measured at 290°C for 200 s. In general, the fading uncorrected post-IR IRSL ages agree with both the quartz OSL and the tephra ages. We conclude that the post-IR IRSL signal from these samples does not fade significantly and allows precise and accurate age determinations on these sediments.     

Optical dating of alluvial deposits at the orogenic front of the andean precordillera (Mendoza,Argentina)

Well constrained numerical ages of alluvial fan sediments are key to understanding the chronology of alluvial episodes and tectonic activity at the front of the Andean Precordillera. We tested the application of radiocarbon and optically stimulated luminescence (OSL) dating in the distal part of an alluvial fan five kilometers north of Mendoza. For OSL dating a large number of aliquots (n > 70) — each composed of ∼50 quartz grains — were measured in order to obtain reliable burial ages despite scattered dose distributions. Owing to a feldspar contamination in all samples, an infrared stimulation was inserted before each OSL measurement, which reduced the feldspar OSL signal successfully. By using the minimum age model we obtained stratigraphically consistent burial ages of alluvial deposits in a depth profile. The uppermost ∼1 m of sediment is composed of debris flow deposits buried 770±76 years ago. Three plant remnants used for radiocarbon dating from the same layer, however, yielded ages younger than 350 years, which are interpreted to underestimate the depositional age. Underneath the debris flow, a major unconformity cuts a series of distal alluvial fan sediments with interstratified floodplain deposits, which are composed of sandy and calciterich silt layers, respectively. Three samples from this unit which were distributed over one meter of sediment thickness yielded statistically concordant OSL ages of 12.3±1.2 ka, 12.3±1.2 ka, and 11.7±1.1 ka. The deposition of these sediments during the latest Pleistocene coincides with a phase of cool and humid climate, which occurred before the alluvial fan propagated farther into the foreland. The overlying debris flow sediments are associated with alluvial fan incision during the arid Late Holocene.     

Thermally assisted OSL: A potent tool for improvement in minimum detectable dose and extension of dose range of Al2O3:C

The influence of electron-phonon interaction on the shape of the optically stimulated luminescence decay curve of Al₂O₃:C has been studied using thermally assisted optically stimulated luminescence (TA-OSL). The minimum detectable dose (MDD) of a phosphor depends on the standard deviation of the background signal which affects the signal-to-noise ratio. The standard deviation of the background signal reduces at lower stimulation light intensity while the readout time increases. Further, measurement at higher temperature enhances the OSL signal with faster decay due to the temperature dependence of photo-ionization cross-section. To achieve the same decay constant and more signal, the temperature of measurement was raised. As a result of lowering the stimulation in-tensity at higher temperature (85°C) the overall MDD of α-Al₂O₃:C was found to improve by 1.8 times. For extension of dose linearity in higher range, deeper traps were studied by simultaneous application of CW-OSL and thermal stimulation up to 400°C, using a linear heating rate of 4K/s. By using this method, two well defined peaks at 121°C and 232°C were observed. These TA-OSL peaks have been correlated with two deeper defects which can be thermally bleached at 650°C and 900°C respectively. These deeper defects are stable up to 500°C, so they can store absorbed dose information even if the sample is inadvertently exposed to light or heat. The dose vs. TA-OSL response from deep traps of α-Al₂O₃:C was found to be linear up to 10 kGy, thus extending its application for high dose dosimetry.     

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.     

FIFTY YEARS OF LUMINESCENCE DATING*

Luminescence techniques for dating both heated materials (e.g., pottery and burnt stone) and sediments have gone through three phases in the past 50 years. The first 22 years, from 1957 to 1979, were devoted to thermoluminescence (TL) techniques applied to heated material. In the next six years, from 1979 to 1985, it was found that TL dating could be applied to sediments. However, the TL signals of both quartz and feldspar grains observed for modern sediments were small, but were not zero, thus making them useful only for older sediments. A new luminescence signal that was totally zeroed by exposure to sunlight for a relatively short period of time, a few hours or less, was found; this led to the development of optically stimulated luminescence (OSL) dating techniques in 1985. Further developments have continued to the present day. Within the past 22 years, 1999 was also a year with major developments. A reliable procedure for single aliquots of quartz that have a rapidly bleached (‘fast’) OSL component was formalized and an instrument that allowed rapid measurement of equivalent doses for single grains was constructed. These developments have led to OSL becoming a major dating tool in Quaternary geology, at least for the past 100 000 years, and in archaeology, particularly as related to the dispersal of modern humans.     

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.     

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.     

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.     

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).     

A high resolution optical dating study of the Mostiştea loess-palaeosol sequence (SE Romania) using sand-sized quartz

We report on SAR-OSL dating of closely-spaced samples from the loess-palaeosol sequence near Mostiştea lake (Danube Plain, SE Romania). We used sand-sized quartz and a SAR protocol that involved a preheat of 10s at 220°C and a test dose cutheat to 180°C. It is shown that these thermal pretreatments isolate a quartz OSL signal that is dominated by the fast component. The behaviour of this signal in the SAR protocol is then documented. The ratio of the measured to given dose tends to lie slightly but systematically above unity (∼5% on average) and the recycling ratio below unity (∼6% on average); for all samples, the recuperated signal is negligible. Within analytical uncertainty, the nineteen optical ages are internally consistent and agree with the predictions from a palaeomagnetic age-depth model. Although it may be possible to optimize the SAR measurement procedure, the optical ages already confirm the chronostratigraphic position of the uppermost welldeveloped palaeosol in that it formed during MIS 5. The established chronology allows correlating the sequence near Mostiştea lake with that near Mircea VodĂ that we investigated earlier.     

Estimation of OSL trap parameters by optical “cleaning” — a critical study

The so-called thermal “cleaning” applied in thermoluminescence analysis allows distinguishing TL signal originating from different traps of comparable thermal depths. Here, the detailed study on the suitability of a similar approach — which can be called optical “cleaning” — for the analysis of OSL process has been carried out by means of computer modelling. The optical “cleaning” is realized by short optical stimulation applied directly after irradiation. It turns out that this approach does not help to separate signals related to various traps having similar optical cross-section (OCS) values. For some sets of trap parameters, sufficiently good reconstruction of the trap optical cross-sections can be achieved by the analysis of the conventional OSL curve obtained directly after sample irradiation, while the OSL curve analysis after “cleaning” does not provide any additional data. For other cases the analysis of both curves with and without “cleaning” leads to optical cross-section values different from those assumed in the model, but just in such situations the optical “cleaning” can be helpful. The differences between the OSL components of the conventional curve and the one obtained after “cleaning” can be used as indicators of an incompatibility of the trap parameters obtained from the OSL analysis with their actual values.     

Different approaches to date bricks from historical buildings

The application of Thermally (TL) and Optically (OSL) Stimulated Luminescence on bricks used as building material has allowed solving an chronological issue in the field of historical building dating. The possibility to use one or more methodologies of dating is closely related to the luminescent and granulometric characteristics of the sample. Using some brick samples collected in the church of Sain Seurin in Bordeaux (France), this paper discusses the implications and the possibility to use different approaches and techniques for dating. With this aim luminescence measurements were performed on both polymineral fine grain and quartz inclusion phases extracted from each brick. For Equivalent Dose (ED) and consequently age determination, TL on mixed fine grain fraction (FG), OSL on quartz inclusions (QI) and on mixed fine grain (FG*) fraction, were used. The results obtained suggest the advantage of using OSL technique on fine grain fraction cleaned up by IR stimulation (FG*), but the use of quartz inclusion represents indeed a good alternative.     

OPTICAL DATING OF GRANITIC STONE SURFACES*

A novel luminescence methodology for dating surfaces of granitoid rocks is presented, with encouraging results for archaeological stone structures. It is based on the zeroing of the latent signal of optically stimulated luminescence (OSL) in feldspar and quartz grains of the stone surface during exposure to daylight. When after bleaching the surface is shielded from light, the OSL signal builds up again, such that its intensity provides an age for the event of the last exposure to light. This event could be the construction or the destruction of stone structures or, for example, sedimentary deposition of granitic boulders, such as in fan deposits. The experimental approach utilizes a high spatial resolution detection technique (HR‐OSL) for OSL of minerals that are left in their original petrological context; that is, without any mineral separation. With this approach, steep gradients in microdosimetry at the surface and at grain boundaries become important and are discussed in detail. The new dating technique is successfully applied to a stone wall of the medieval castle of Lindenfels in southwestern Germany and the pre‐Columbian Nasca lines (geoglyphs) around Palpa in southern Peru.     

New radiometric ages for the Early Upper Palaeolithic type locality of Brno-Bohunice (Czech Republic): comparison of OSL,IRSL, TL and C dating results

New radiometric data are reported from the recent excavation of the type locality of the Early Upper Palaeolithic entity of the Bohunician. Recently obtained radiocarbon (¹⁴C) data on charcoal are compared with new Optically Stimulated Luminescence (OSL) dating of sediment. OSL ages were determined on sediment from the archaeological occupation at Brno-Bohunice, as well as from the over- and underlying loessic sediments. Multiple techniques were applied, which all gave congruent results. While a dual protocol (post IR-OSL) failed the quality criteria tests, ages were obtained by Multiple-Aliquot-Additive-Dose (MAAD) on polymineral material and Single-Aliquot-Regeneration (SAR) on fine grain quartz extract as well as on polymineral material. Fading tests show significant loss of Infrared Stimulated Luminescence (IRSL) after storage for 3 and 12 months for one sample, but little or no fading for others. The resulting (uncorrected) age estimates are smaller than those on quartz by OSL methods. The latter are considered to be more reliable estimates of the sedimentation age of these deposits. The measured OSL doses do not show a simple distribution and the lowest 5% was used for age calculation to represent the most likely sedimentation age. The quartz from the loess overlying the archaeological layer is OSL dated to 30.9 ± 3.1 ka, while the sediment for the paleosol which contains the archaeological layer gave an age of 58.7 ± 5.8 ka. The attribution of this paleosol to the Hengelo interstadial is therefore questionable. However, if the Hengelo interstadial is correlated with the Dansgaard/Oeschger (D/O) event 12, statistical agreement within 2-σ is achieved. The OSL result for the archaeological layer is in accordance with a weighted average TL date on heated flint artifacts of 48.2 ± 1.9 ka from this layer as well as calibrated radiocarbon data (CalPal Hulu 2007) from nearby locations. However, radiocarbon data on charcoal samples obtained during excavation at Brno-Bohunice 2002 provide age estimates between 30 and 40 ka ¹⁴C-years, which translate to approximately (33) 35–44 ka on the calendric time scale according to the Hulu 2007 model. For the underlying loess a depositional age of 104.3 ± 10.6 ka was obtained by OSL. The presented OSL ages indicate that a simple correlation of soil sequences between sites within a region has to be verified by chronometric dating.     

An assessment of the luminescence sensitivity of Australian quartz with respect to sediment history

This study provides a preliminary systematic characterisation of OSL sensitivity, with respect to sediment history, of single grains of Australian quartz from a variety of source rocks and depositional contexts. Samples from two distinct lithologies and with relatively short modern sedimentary histories were compared in an examination of the influence of rock type on OSL sensitivity. Sediments derived from weathered sandstone were found to be brighter than those from metamorphosed schists, suggesting that sensitivity may be inherited from the source rock and its earlier sedimentary history. Secondly, quartz from the same source, but different modes of deposition, was compared to assess the effect on sensitivity of nature of exposure to light during the most recent bleaching event. Quartz grain sensitivity appears not to vary depending on the mode of sediment deposition, suggesting that the nature of exposure to light during deposition is less important in the sensitisation process. This study highlights the complexity and variety of natural sedimentary quartz, demonstrating the limitations of an investigation based solely on OSL sensitivity. Further systematic investigation into the physical, geological and geomorphological characteristics of sediments is proposed to better understand the mechanisms of luminescence sensitisation in 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.     

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.