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.     

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.     

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.     

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.     

A contribution to the study of post-depositional alterations of pottery using TL dating analysis

In luminescence dating, the potassium concentration significantly contributes to the dose rate value in the age estimation. Within this study, fine-grain thermoluminescence dating has been applied on sherds of calcareous pottery of known age, excavated at a Roman site in Mallorca, Spain. For those of the samples that showed signs of severe potassium leaching, according to chemical and mineralogical examination, the thermoluminescence analysis provided overestimated dates. By using the known archaeological age of the samples, a corrected dose rate value can be estimated which provides the potassium concentration averaged for the burial period. Finally, a step-like model can then be used to estimate the fraction of the burial period after which most of the alteration effects took place.     

Surface dating by luminescence: An overview

Daylight radiation resets luminescence ‘clock’ to zero on rock surfaces, but transmission depends on the transparency of the rock. On burial, surfaces are no longer exposed to daylight and accumulation of trapped electrons takes place till the excavation. This reduction of luminescence as a function of depth fulfils the prerequisite criterion of daylight bleaching. Thus rock artefacts and monuments follow similar bleaching rationale as those for sediments. In limestone and marble, daylight can reach depths of 0.5–1 mm and up to 16 mm respectively, while for other igneous rocks e.g. quartz in granites, partial bleaching occurs up to 5mm depth under several hours of daylight exposures and almost complete beaching is achieved in the first 1 mm within about 1 min daylight exposure. The ‘quartz technique’ for limestone monuments containing traces of quartz enables their dating with Optically Stimulated Luminescence (OSL) techniques. The surface luminescence (thermoluminescence, TL or OSL) dating has been developed and further refined on various aspects of equivalent dose determination, complex radiation geometry, incomplete bleaching etc. A historical review of the development including important applications, along with some methodological aspects are discussed.     

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.     

一对青花云龙纹象耳瓶热释光年代测定报告

应用前剂量饱和指数法对两件青花云龙纹象耳瓶瓷器作了热释光年代测定,得到这两件瓷器的烧制年代均小于距今100年,否定了成份分析法得到的这两件瓷器系元代真品的错误结论。     

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.     

Thermoluminescence as a technique for determining the nature and history of small solar system particles

The thermoluminescence phenomenon has been used for pottery dating and radiation dosimetry for sixty years and for forty years has been applied to the study of meteorites, being successful in quantifying metamorphic histories and providing new insights into terrestrial age and orbits. Here we review some of the fundamental properties of thermoluminescence with particular focus on the study of small extraterrestrial particles. We suggest that natural TL data can be used to identify the burial and release history of cometary particles and that induced TL measurements can provide in-sights into the mineralogy of particles (even when largely amorphous) and the metamorphic history of those particles. We illustrate the use of TL to study small particles by describing recent studies on micrometeorites and 10–100 μm fragments taken from the matrix of a meteorite Semarkona which is type 3.0 ordinary chondrite.     

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

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

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

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

Decline in firing technology or poorer fuel resources? High-temperature thermoluminescence (HTTL) archaeothermometry of Neolithic ceramics from Pool,Sanday, Orkney

The Neolithic ceramic assemblage from the multi-period coastal settlement at Pool on the island of Sanday, Orkney is unique because it stratigraphically spans both the earlier round-based (including possible Unstan bowls) and later flat-based (‘Grooved Ware’) traditions. High-temperature thermoluminescence (HTTL) analysis objectively demonstrates that ceramics from the earliest Neolithic layers have been consistently better fired compared to examples from later layers. We suggest two interpretations of these data: either firing technology declined with changing social structures and/or adoption of a different ceramic tradition or that there was greater pressure on fuel resource and management in the later Neolithic. Paleoenvironmental and chronological evidence indicate climatic deterioration in the later Neolithic, which adds further support to an interpretation of a poorer fuel resource at that time. In addition to studies of the HTTL signal, analysis of the ambient temperature modification of the TL signal has potential to support or evaluate dating evidence, and is readily applicable to optically stimulated luminescence (OSL) age data.     

The Firing Temperature of Pottery from Ancient Mesopotamia,Turkey, Using Luminescence Methods: A Case Study for Different Grain‐Size Fractions

The assessment of the firing temperature of a prehistoric pottery sample collected from ancient Mesopotamia, Turkey was studied using luminescence techniques. The methods for this estimation involved the observation of the thermal and pre‐dose sensitization with various re‐firing temperatures for both TL and the OSL signals. In the former case, the 110°C TL peak and the rest of the glow curve were used as proxies in this study. In the framework of a first attempt to investigate the impact of grain‐size dependence on the sensitization of the luminescence signals, the aforementioned study was performed with four different pottery grain‐size fractions: (i) less than 60 μm, (ii) 60–90 μm, (iii) 90–180 μm and (iv) 180–250 μm. The results clearly demonstrated the firing temperature mark of ～500°C in for the grain size of 90–180 μm, while—as in the case of the lower grain‐size fraction—a third proxy, the ratio of the pre‐dosed to the thermal sensitization, was seen to indicate the firing temperature. The remaining two grain‐size fractions failed to provide any meaningful results with regard to the firing temperature estimation. The dependence of the TL characteristics on the grain size was explained in the framework of the mixed mineralogy.     

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.     

Kinetic analysis of thermoluminescence glow curves in feldspar: evidence for a continuous distribution of energies

The thermoluminescence (TL) glow curves from feldspars have been the subject of numerous studies, because of their importance in luminescence dating and dosimetry. This paper presents new experimental TL glow curves in a plagioclase feldspar, measured using the T _max-T _stop technique of glow curve analysis. Kinetic analysis of the experimental results is carried out for a freshly irradiated sample, as well as for a sample which has undergone optical treatment using infrared light for 100 s at 50°C. Application of the initial rise method of analysis indicates that the TL signals from both samples can be characterized by a continuous distribution of energy levels. By subtracting the TL glow curves measured at successive T _stop values, a series of TL glow curves is obtained which are analyzed using the empirical general order kinetics. It is found that all TL glow curves obtained by this subtractive procedure can be described accurately by the same general order parameter b ～1.7. In a second attempt to analyze the same TL glow curves and possibly extract information about the underlying luminescence process, the shape of TL glow curves is analyzed using a recently proposed physical kinetic model which describes localized electronic recombination in donor-acceptor pairs. Within this model, recombination is assumed to take place via the excited state of the donor, and nearest-neighbor recombinations take place within a random distribution of centers. This recent model has been used recently to describe successfully several types of luminescence signals. This paper shows that it is possible to obtain good fits to the experimental data using either one of these two approaches.     

DETECTION OF ANCIENT MARBLE FORGERY: TECHNIQUES AND LIMITATIONS*

Since 1960, scientific results have replaced aesthetic judgements in marble authentication studies and the technology to perform analytical tests on micro‐samples has developed rapidly. However, no single method can be used to determine the authenticity of a piece of marble. A ‘detective‐like’ investigation is usually adopted by using optical microscopy, ultraviolet‐induced fluorescence, provenance determination techniques and mineralogical, chemical and morphological analyses of the patina. A newly proposed thermoluminescence methodology calculates the ‘burial age’ of recently excavated objects or distinguishes artefacts exposed to sunlight since antiquity from those exposed recently. The technique shows a lot of potential; however, much work remains to be done.     

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.     

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.     

The Potential for Dating the Old Scatness Site,Shetland, By Optically Stimulated Luminescence

A series of deposits from the agricultural infield of the multiperiod settlement mound, Old Scatness, were investigated for their potential to yield optically stimulated luminescence dates. Luminescence properties of quartz grains were found to vary through the sequence, but dates were successfully obtained from five deposits, including anthropogenic soils, windblown sands and sands within midden deposits. Single‐aliquot equivalent dose measurement was found to be the most appropriate method for dating the deposits. The OSL dates obtained accorded well with the dates provided by archaeological evidence and included the post‐medieval, Iron Age, Bronze Age and Neolithic periods of Shetland, while a substantial midden was dated to the Bronze/Iron Age transition.