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.     

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.     

Dating mortar by optically stimulated luminescence: A feasibility study

Quartz is the datable component in mortar. Although its luminescence properties are very well studied, the problem of mortar dating arises from a low level of optical bleaching. In order to reduce the time consuming efforts for dating lime mortar in monuments by optically stimulated luminescence, we investigated the most suitable methods of dose and dose rate determination, and we explored tests which are suitable to predict the datability of a given material. Reverting to the large number of publications on sedimentary partially bleached quartz we found linear modulation techniques especially useful, equally we also recommend the determination of the level of optical depletion before starting analyses. Single grain analysis is regarded as an ultimate but infallible tool to date very poorly bleached quartz from mortar. Dose rate measurements need to take into account the radioactive equilibrium of the uranium decay and the short range inhomogeneity of the environmental gamma radiation field: gamma spectrometry and on-site TLD measurements are best suited.     

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.     

A review of rock art dating in the Kimberley, Western Australia

This paper critically reviews the various approaches used to estimate the age of the rock art in the Kimberley region of Western Australia. They include: (i) the relative superimposition of styles; (ii) the use of diagnostic subject matter (depictions of extinct animals, stone tool technology, introduced European and Asian objects and animals); (iii) the recovery of a ‘painted’ slab from a dated archaeological unit; (iv) radiocarbon dating of beeswax figures, charcoal pigments, organic matter in overlying mineral deposits and ‘accreted paint layers’ (oxalate rich crusts and amorphous silica skin), pollen grains from an overlaying mud-wasp nest; and (v) optically stimulated luminescence (OSL) dating of quartz grains from overlying mud-wasp nests. Future directions for rock art dating in the Kimberley include uranium-series dating of overlying and underlying mineral deposits.     

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.     

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.     

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.     

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.     

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.     

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.     

METHODOLOGICAL DEVELOPMENTS IN THE LUMINESCENCE DATING OF BRICK FROM ENGLISH LATE‐MEDIEVAL AND POST‐MEDIEVAL BUILDINGS*

Fired clay brick samples, obtained from a group of seven high‐status late‐medieval and post‐medieval buildings in England ranging in age from c. ad 1390 to 1740, were dated by the luminescence method using an optically stimulated luminescence (OSL) technique. The results obtained indicate that, when applied to quartz extracted from brick, the technique is capable of producing dates that are in consistently good agreement with independent dating evidence for the buildings. For six samples taken from a group of four dating ‘control’ buildings the mean difference between the central values of luminescence and assigned ages was 5 ± 10 years (SD, n = 6). The methodology used is appropriate for application to other standing buildings in other temporal and geographic regions, and may be used with confidence where conventional dating methods are less certain. The study also examines the luminescence characteristics of quartz and the characteristics of the lithogenic radionuclides in brick samples and identifies various aspects related to the assessment of experimental uncertainty in testing the reliability of the method.     

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.     

Luminescence Dating of Monumental Stone Architecture at Chavín De Huántar,Perú

Optically stimulated luminescence (OSL) is applied to quartz extracted from mud mortar collected from Chavín de Huántar, an early Andean monumental center. The samples appear to have been only partially exposed to sunlight during construction, so a minimum age model is applied to equivalent dose distributions. Complications, including complex radioactivity, low sensitivity of the quartz, and limited sample, prevent high precision, but the 14 dates obtained cluster around 1000 BC largely in agreement with radiocarbon assays on charcoal also collected from the mortar. Results suggest a relatively rapid construction for the monument. This work develops OSL as a method for directly dating architectural mortar.     

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.     

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.     

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.     

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.     

Luminescence geochronology and paleoenvironmental implications of coastal deposits of southeast Cyprus

Quaternary stratigraphy and sea level changes have been extensively investigated in many areas of the Mediterranean. However, numerical dating of coastal deposits and the associated paleoenvironmental information are limited for the coasts of Cyprus, principally based on radiometric and radiation-exposure geochronological techniques on fossils which bear a range of limitations and uncertainties. As such, optically stimulated luminescence (OSL) dating techniques are deemed to be the most suitable in direct dating of the coastal sediments of Cyprus. In the southeastern Cyprus, coastal dunes (aeolianites) now forming elongated ridges appear as morphological features running parallel to the current shoreline presenting an indicator of sea level and climate changes of great paleoenvironmental significance. We present our first chronological results for the exposed aeolianites and underlying littoral deposits formed along the southeastern coastal Cyprus ranging from 78.4 ± 9.9 to 56.2 ± 7.4 ka. The post-infrared–infrared stimulated luminescence (pIR-IRSL) revealed that dune formation took place during the marine isotope stages (MISs) 3, 4, and possibly 5a. Late Holocene reworking is proposed for a distinctively isolated dune with an age of ~1.3 ka ago. This study also showed that pIR-IRSL dating of feldspars may be a reliable alternative to quartz OSL dating when the quartz luminescence characteristics are unsuitable.     

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.