Natural IRSL intensities and apparent luminescence ages of single feldspar grains extracted from partially bleached sediments

The single aliquot technique has been applied to single grains of K-feldspar extracted from a well-dated late-glacial marine sediment sample for which standard luminescence dating yielded ages that were in excess of the expected age. Natural infrared-stimulated luminescence (IRSL) intensities as well as single grain palaeodoses show a wide range of values. Most of the bright grains yield equivalent doses largely in excess of the expected palaeodose, considering the depositional age of the sample. The luminescence emitted by the brightest grains would dominate the signal emitted from aliquots containing many grains. This explains the overestimation of ages obtained using standard luminescence techniques for the sample investigated. Palaeodoses obtained from grains that exhibit low IRSL intensities are close to the expected dose. However, the age derived from these grains is lower than the expected age. Anomalous fading is believed to be the main cause for the age underestimation. This study is the first demonstration of the feasibility of dating a sedimentary event using the luminescence of a single mineral grain.     

Behavioural studies of stimulated luminescence from feldspars

Since the work of Mejdahl in the mid-1980s feldspars have been used widely for palaeodosimetry. They have proved particularly popular because of the technical ease with which an optically stimulated luminescence signal can be obtained, and the potential for their use in dating over a wider time range than quartz. However, while the use of infrared stimulated lminescence has been a great success, the realisation of the potential for dating over a wide time range has been hampered by a series of behavioural problems, in particular concerned with the stability of the luminescence signal. This paper surveys the current state of knowledge of a range of aspects of the stimulated luminescence behaviour of feldspar. Particular attention is paid to the thermal and optical properties of the thermoluminescence (TL) and optically stimulated luminescence (OSL) signals from feldspars since these are of greatest relevance to their use as palaeodosimeters. Results obtained from well-characterised museum specimens demonstrate the variety of responses that are seen from different types of feldspar, particularly in their TL behaviour. Less variation is seen in their OSL response. In contrast, the response of potassium-rich feldspars separated from Quaternary sediments tends to be very consistent when many grains are analysed simultaneously, suggesting that averaging of the signal simplifies the behaviour of the system.     

Natural luminescence and anomalous fading in K-feldspar

This study investigated the relationship between the natural luminescence intensity, the amplitude of anomalous fading and the apparent IRSL age of a suite of feldspar single grains. Correlating natural luminescence with fading may simplify the identification of weakly to non-fading feldspars grains in sediments. In our single grain experiments, the mean fading corrected IRSL age obtained from a small population of bright grains is close to the expected depositional age of the sediment investigated. It is proposed that in dating programs, more attention should be given to bright feldspar grains as they are the most stable grains in the population.     

A new irradiated quartz for beta source calibration

For luminescence dating to be an accurate absolute dating technique it is very important that we are able to deliver absolutely known radiation doses in the laboratory. This is normally done using a radiation source (alpha, beta, X-ray) calibrated against an absolutely known reference source. Many laboratories have used the various different batches of Risø calibration quartz for the calibration of beta and X-ray sources, but these have been largely undescribed. Here we describe in detail the preparation and luminescence characteristics of a new quartz standard, based on a North Sea beach sand collected from south-western Denmark (Rømø). Two grain sizes (4–11 μm and 180–250 μm) have been examined in detail. These were pre-treated (annealed, dosed and annealed again) to sensitise and stabilise the luminescence signals before being given an absolutely known gamma dose from a point ¹³⁷Cs source in scatter-free geometry. The luminescence characteristics are described; the very intense blue-light stimulated signal is dominated by the fast OSL component and the IR-stimulated signal is negligible. The material is shown to be suitable for measurement using SAR, and the dose recovery ratio is indistinguishable from unity with a standard deviation of <2% for multi-grain aliquots. The material is also shown to be suitable for single-grain calibration, with >80% of the grains giving a useful signal. Although there is an unexplained dispersion in our calibration data of ∼3% (which we cannot attribute to instrument variability), we nevertheless conclude that this material is very suitable for transferring absolute known doses from a standardised gamma source to in-built irradiation sources.     

Luminescence dating: laboratory procedures and protocols

In the last 30 years, from 1967 to 1997, the use of luminescence signals from naturally occurring minerals has gone though a major metamorphosis, from thermoluminescence (TL) dating of pottery to optically stimulated luminescence (OSL) dating of sediments. Laboratory procedures for dating sediments have been adapted from those for pottery and new procedures have been developed as the need arises.

The majority of sediment dating applications are carried out on quartz and potassium-rich feldspars and the general characteristics of the TL and OSL signals from these minerals are reviewed. For sediments some new problems were encountered, with some grains perhaps not being completely bleached at deposition. For OSL signals there is no simple procedure for the selection of a thermally stable signal, as there had been in the case of pottery.

Many different laboratory protocols have been developed as our understanding of the fundamental behaviour of luminescence signals from quartz and feldspar has improved. These protocols are explained and discussed, giving the advantages and disadvantages of each procedure as applied to different types of sediment.

This review is presented as a guide to the selection of the most appropriate procedure for a particular dating application.     

Optically stimulated luminescence production in the single-aliquot regenerative dose protocol

When using a single-aliquot regenerative dose (SAR) protocol for luminescence dating of sedimentary quartz grains, the fundamental assumption is that the sensitivity of the optically stimulated luminescence (OSL) produced by the regenerative doses can be monitored by their following test dose OSL response. Using well-bleached coarse quartz grains, OSL production in a SAR protocol was studied in detail when dose response curves were constructed using both single and multiple aliquot regenerative dose procedures. During application of the SAR protocol, two preheats are applied, each ahead of an OSL measurement that is produced by the regenerative dose and test dose, respectively. It is shown that sensitivity changes caused by heating were well corrected for using the OSL response to the test dose. However, these preheats are shown to result in thermally stimulated OSL signals that contribute both to the OSL response from the regenerative doses used to construct the dose response curve and to the OSL response from the test dose used to monitor OSL sensitivity changes as the quartz grains are repeatedly measured. A simple test is proposed to identify the contribution of the latter signal.     

Dosimetric properties of natural quartz grains extracted from fired materials

The paper describes an examination of the dosimetric properties of natural quartz grains extracted from ancient fired materials. Eleven samples of different origin were tested for their TL and GLSL (green light stimulated luminescence) sensitivities within the mGy dose range. Very promising results were obtained showing the possibility of measuring the doses of around 10 mGy with 1% precision using GLSL or TL and using the single aliqout technique for natural quartz as a dosimeter. The lowest detectable dose was estimated to be lower than 500 μGy. The results obtained indicate that natural quartz grains from selected materials could be used for the dosimetry of environmental gamma radiation for the purposes of paleodosimetric dating methods as well as for accident dosimetry.     

Mineral zircon: A novel thermoluminescence geochronometer

Mineral zircon contains trace amounts (typically 10-1000 v ppm) of the f -emitters uranium and thorium, which irradiate this mineral internally. This outstanding feature of zircon turns out to be extremely useful when this mineral is applied as a thermoluminescence (TL) dating medium, because the build-up of the age-dependent luminescence is dominated by the presence of well-defined internal radioactive sources and the contributions to the dose from external radiation sources are two orders of magnitude smaller. The results presented in this paper have led us to the conclusion that for zircon dating it is necessary to carefully select the best and homogeneous zircon grains of the highest optical quality. For successful dating experiments on very young and historically well-defined coastal dune sands, selection of the most stable luminescence component by means of narrow band interference filters is needed. Our results suggest that ultimately optical zircon dating will allow us to determine the age of extremely young samples ( e.g. 12 months!).     

Facets of Luminescence for Dating

The aim of this article is to introduce luminescence dating and relate it to luminescence and Raman spectroscopy of minerals. The physical bases of luminescence signals used in dating and their relationships to other radiation-induced luminescence and Raman signals are briefly reviewed. The manner in which these signals are applied to evaluate luminescence ages is described. Archaeological and geological case studies from the author's experience are used to illustrate potentialities and issues related to different contexts, techniques, and materials.     

Determining the K-content of single-grains of feldspar for luminescence dating

Feldspars form a solid-solution series whereby the K-content may range from 0 to 14%. LA-ICP-MS measurements for density-separated single-grains of feldspar yielded realistic concentrations of K within the range of those naturally occurring, and also highlighted the difficulty in isolating the pure end members during density-separation. No direct relationship was found between the thermal stability of the infrared-stimulated luminescence (IRSL) signal and measured K-content of individual grains. However, the brightest IRSL and post-IR IRSL signals originated from grains with ～12% K-content. All grains giving a measurable signal had K-content between 6 and 13%, therefore it is suggested that an internal K-content of 10 ± 2% can be assumed for routine single-grain dating of density-separated K-feldspars.     

Variations in luminescence properties of single quartz grains and their consequences for equivalent dose estimation

In this paper examples of variability of luminescence properties between single grains of quartz extracted from natural samples or from crushed single crystals are shown. It is demonstrated how measurements of glow curves, PSL (photon stimulated luminescence) decay curves, thermal activation characteristics using multi-grain aliquots can lead to a misinterpretation of the obtained data. The possible consequences for different D_E estimation techniques applied to multi-grain aliquots or to single grains and normalisation techniques applied to multi-grain aliquots are discussed. In particular pre-dose, multi-aliquot additive, and single grain PSL SAR D_E estimation methods are considered.     

Spectral information from minerals relevant for luminescence dating

The paper reviews basic spectral features of luminescence from minerals used in dating and allied research. Luminescence production is a result of multiple interactions within the imperfect crystal lattice and spectral information is not limited to the emission of light. Results of spectral investigations of luminescence emission during thermal stimulation (TL) or optical stimulation (OSL) form the main part of the paper. However, information on luminescence excitation and light absorption spectroscopy is also presented and possible links between luminescence production in minerals and particular lattice defects are considered. Quartz and feldspars, the most commonly used minerals, receive special attention, but the review includes other materials such as polymineral fine-grained fractions from sediments, zircon, calcite and other salts (halite, sulfate), meteorites, flint, volcanic materials (obsidian, tephra), ceramics and metallurgical slags. Although a wide range of different luminescence emission wavebands occur, it can be shown that certain emissions dominate in particular materials. Basic dosimetric properties are often known just for single emission wavebands of a particular mineral, and are listed in this case. The paper also aims to provide a starting point and inspiration for the study of other TL and OSL emissions, with particular regard to their potential and suitability for dating and related dosimetry tasks. These investigations, involving palaeodose determination based on an emission waveband with known characteristics, need careful separation of the particular emission peak, which may be influenced by its behaviour during the dating procedure (sample preparation, irradiation, preheat treatments, luminescence measurements, etc.). Spectral information available in this context and some technical remarks on the experimental conditions will be given to pave the way for conventional TL or OSL measurements in luminescence dating and dosimetry using natural or semi-natural materials.     

Optical dating of single sand-sized grains of quartz: sources of variability

Optically stimulated luminescence (OSL) measurements have been made of over 3000 sand-sized grains of quartz. Analysis at this scale highlights the variability in the luminescence sensitivity and the dose saturation characteristics of individual quartz grains. Using a new instrument capable of measuring single grains it is feasible to routinely measure the equivalent dose from many hundreds of grains from each sample. Analysis of such datasets requires assessment of the uncertainties on each equivalent dose since these may vary significantly. This paper assesses the significance of signal intensity, dose saturation characteristics and instrument uncertainty in equivalent dose calculation.     

The dependence of quartz OSL on stimulation energy

Quartz is the mineral most commonly used for sediment dating. In dating practice, the optically stimulated luminescence (OSL) of quartz is measured mainly using the stimulation light whose wavelength is 470 ± 30 nm. The parameters of traps active in the OSL process are also determined for this stimulation band. The zeroing of the OSL is the fundamental condition of applicability of the luminescence dating for specific sediment and takes place in sunlight whose spectrum differs significantly from the band 470 ± 30 nm. In order to be able to know the course of OSL process in nature, a wider knowledge of the dependency of the trap parameters on the stimulation band is needed. Here the results are presented for the OSL measurements carried out with different wavelengths of stimulation light. For each stimulation band the components of the OSL signal are determined by the fitting procedure, and in this way the wavelength dependence of an individual component is found. The experiment has been repeated for two temperatures of OSL detection – the room temperature, which corresponds to natural conditions, and for 125 °C, which is the temperature usually applied for OSL measurement in dating. Four OSL components are presented in both experimental series. The values of their optical cross-section changes along with stimulation energy and temperature, as it is predicted by the model of OSL process including crystal lattice vibrations.     

Assessment of diagnostic tests for evaluating the reliability of SAR De values from polymineral and quartz fine grains

In this study, we applied optically stimulated luminescence (OSL) dating to two fine grain sediment samples collected at Jeongokri, Korea. A single aliquot regenerative dose (SAR) procedure was applied to both polymineral grains and to chemically isolated (H₂SiF₆) quartz grains of 4–11 μm diameter. For polymineral fine grains, the OSL IR depletion ratio and the equivalent dose (D_e) plateau test appear to be equally sensitive indicators of appropriate IR stimulation time for use in the ‘double SAR’ protocol. Additionally, the OSL IR depletion ratio test gives an indication of the relative mineral composition of the samples, hence providing an assessment of the likelihood of obtaining a quartz-dominated [post-IR] OSL signal. Use of higher preheat temperatures would assist in thermally eroding the non-quartz component of the [post-IR] OSL signal from polyminerals. For the quartz fine grains, data from both natural D_e determinations and laboratory dose recovery tests are required to identify the appropriate preheat temperatures for dating, due to problems of thermal transfer. This phenomenon is particularly exaggerated for these samples due to the large D_e values (≥350 Gy) and hence low slope of the dose–response curve. The double SAR method cannot be applied ubiquitously, even after careful and rigorous study of one sample from a section. Quartz OSL dating using a range of preheat temperatures is suggested to be the most suitable method for OSL dating of fine grain sediments.     

Dating bricks of the last two millennia from Newcastle upon Tyne: a preliminary study

Bricks from a group of four independently dated late medieval buildings in Newcastle upon Tyne have been tested to establish their suitability for luminescence dating as part of a wider study of the dating of post-Roman and medieval brick buildings. The luminescence characteristics of quartz extracted from the bricks were determined using TL (210°C peak) and OSL measurement procedures. Both TL and OSL measurement procedures based on SAR and SARA protocols were applied to determine the palaeodose. The luminescence dates for three sampled locations are in good agreement with the assigned architectural dates; the fourth appears to be older raising doubts concerning the architectural assessment of the sampled phase.     

Steps towards surface dating using luminescence

Whereas luminescence dating applications usually avoid gradients and therefore surfaces, this study explores the requirements and possibilities of dating surfaces using infrared stimulated luminescence. The basic prerequisite for dating applications is a dose-dependent, bleachable and stable luminescence signal. It was found to be fulfilled for crushed granite rock material. Depth profiles below polished surfaces of granites indicate that a well bleached layer below the actual surface solely contributes to the infrared stimulated luminescence signal. A new measurement device, designed for in situ surface dating applications, is presented along with first experimental results.     

The fadia method: a new approach in luminescence dating using the analysis of single feldspar grains

The fadia method has been recently introduced in luminescence as one that may potentially resolve the problem of anomalous fading and age shortfalls in IRSL dating of sediments. This method takes advantage of the differential fading rates of single feldspar grains and allows one to extrapolate to zero fading. This paper describes step by step the protocol used in the Montréal laboratory. The application of the method is shown to be hampered by the occurrence of faintly luminescent feldspar minerals, and/or unbleached grains in the dated sediment samples.     

Sources of overdispersion in a K-rich feldspar sample from north-central India: Insights from De,K content and IRSL age distributions for individual grains

Luminescence dating of individual sand-sized grains of quartz is a well-established technique in Quaternary geochronology, but the most ubiquitous mineral on the surface of the Earth—feldspar—has received much less attention at the single-grain level. In this study, we estimated single-grain equivalent dose values and infrared stimulated luminescence (IRSL) ages for K-rich feldspar (KF) grains from a fluvial sample underlying Youngest Toba Tuff (YTT) deposits in north-central India, and compared these ages (corrected for anomalous fading) with those obtained from individual grains of quartz from the same sample. Both minerals have broadly similar single-grain age distributions, but both are greatly overdispersed and most grains have ages substantially younger than the expected age of the YTT deposit (～74 ka). Almost half (45%) of KF grains used for age calculation have fading rates statistically consistent with zero, but the age distribution of these grains is as dispersed as that of the entire population. We obtained a similar distribution of ages calculated for 51 grains using their individually measured internal K contents, which exhibited only minor grain-to-grain variation. Given the lack of dependency of single-grain ages on the measured fading rates and internal K contents, and the overall adequacy of bleaching of grains collected from a sandbar in the modern river channel, we consider the spread in ages is most likely due to mixing, at the time of deposition and after the YTT event, of potentially well-bleached fluvially-transported sediments with older grains derived from slumping of riverbank deposits. Some spread may also be due to natural variations in the IRSL properties of individual KF grains.     

Song of the dunes as a self-synchronized instrument

Since Marco Polo it has been known that some sand dunes have the peculiar ability to emit a loud sound with a well-defined frequency, sometimes for several minutes. The origin of this sustained sound has remained mysterious, partly because of its rarity in nature. It has been recognized that the sound is not due to the air flow around the dunes but to the motion of an avalanche, and not to an acoustic excitation of the grains but to their relative motion. By comparing singing dunes around the world and two controlled experiments, in the laboratory and the field, we prove that the frequency of the sound is the frequency of the relative motion of the sand grains. Sound is produced because moving grains synchronize their motions. The laboratory experiment shows that the dune is not needed for sound emission. A velocity threshold for sound emission is found in both experiments, and an interpretation is proposed.