Influence of pre-measurement thermal treatment on OSL of synthetic quartz measured at room temperature

Much effort has been made to study the influence of pre-measurement thermal treatment and ionizing radiation on quartz specimens owing to its use in a large number of applications. Optically stimulated luminescence (OSL) being a structured and sensitive phenomenon promises to correlate the responsible color center and luminescence emission. OSL studies on quartz with such conditions can reveal many significant results.The aim of the present investigation is to understand the effect of annealing temperature on OSL characteristics of synthetic quartz recorded at room temperature. At identical annealing duration and β-dose, the shape of OSL decay curve remains non-exponential; when specimens annealed at lower temperature (∼400 °C). The shape of decay curve changes to exponential in nature along with rise in OSL intensity when the specimen was given higher temperature of annealing (>400 °C). The effects of such protocol on pattern of OSL sensitivity as well as area under the OSL decay curve are also presented here. The presence of shallow traps, when OSL decay curve was recorded at room temperature seems to be responsible for the changes in OSL pattern. The influence of shallow traps is attributed to non-exponential decay of OSL recorded at room temperature.     

Study of sensitivity change of OSL signals from quartz and feldspars as a function of preheat temperature

Optically stimulated luminescence (OSL) signals from feldspar and quartz samples were studied using infrared (860 nm) and green light (420–575 nm) stimulation. A serious problem connected with the regeneration technique used for dating is associated with a change of OSL sensitivity to radiation in the course of the measurement process. A typical effect seen is a large increase of the apparent strength of our beta source when calibrated against a gamma source. If the regeneration procedure is used, it is shown that the sensitivity increases up to 50% during the measurement process and as a result, the equivalent dose (ED) would be underestimated. A study of sensitivity changes in feldspars and quartz was carried out with emphasis on the effect of preheat and annealing on the OSL signal. Measurement results obtained are presented, and possible elimination of errors in dating caused by sensitivity changes is discussed.     

How to visualize quartz OSL signal components

The optically stimulated luminescence (OSL) signal of natural quartz measured under constant stimulation power (CW-OSL) is a featureless decay curve where underlying components cannot be identified easily. Visual interpretation of quartz OSL signals is easier if signals are shown in spectrum-like form. This can be achieved either through ramped stimulation, or by transforming a measured CW-OSL curve into a pseudo OSL curve. We show that both give similar results, but that transformation should be preferred as CW-OSL provides best signal-to-noise ratios. We present different transformation methods to obtain pseudo OSL curves and discuss the advantages and disadvantages of each method. In addition, we show that different pseudo OSL transformations can be used to emphasize specific aspects of the OSL signal. We conclude that transformation of CW-OSL to pseudo hyperbolically modulated OSL provides the most useful visualization of the quartz fast OSL component. Pseudo parabolic modulated OSL is the transformation of choice for showing the slow component(s). The pseudo OSL curves can be used for rapid visual inspection of the relative contribution of the OSL components prior to further analysis.     

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.     

The timing of OSL sensitivity changes in a natural quartz

The timing of 110°C thermoluminescence (TL) and optically stimulated luminescence (OSL) sensitivity changes is explored using a natural (aeolian) quartz sample from Australia that was previously found to exhibit marked dose-dependent sensitivity change. The changes occur asynchronously; the 110°C TL sensitivity changes after dosing plus pre-heating, whereas the OSL sensitivity changes (proportionately with dose) after optical bleaching. Although the magnitude and saturation characteristics of the sensitivity changes are found to be similar, their non-synchronicity negates a direct link between the phenomena. Implications of these results for dating procedures are discussed. In particular, the results indicate that a single aliquot additive dose procedure similar to that developed for coarse-grained potassium feldspar should be possible for some quartz samples.     

Analysis of optical bleaching of OSL signal in sediment quartz

The aim of this work was to study the effect of the quality of optical bleaching on the results of OSL (Optically Stimulated Luminescence) dating method. The large aliquots of coarse quartz grains extracted from fluvial deposit were used in the study. The poor, medium and good bleaching were simulated in laboratory with help of Blue LED light source in series of experiments. Then the samples were irradiated with a common laboratory dose. The equivalent doses (DE) were measured by the help of standard Single Aliquot Regeneration (SAR) technique, but obtained DE distributions are analyzed in a new way. The method for recognizing and compensating for partial bleaching is proposed. The conclusions for dating sediment quartz samples are presented and discussed.     

Zeroing of the OSL signal in quartz from young glaciofluvial sediments

The natural luminescence of quartz samples from recent (<200 yr old) glaciofluvial sediments collected from a range of distances from the snout of the Gangotri glacier in the Garhwal Himalaya, India, was measured. Six measured D_E (equivalent dose) values ranged from 35 to 175 Gy, strongly suggesting that these samples had been exposed to daylight only poorly before deposition. However, regenerated growth curves constructed after exposure to several hours of natural daylight gave apparent D_E values ranging from 10 to 30 Gy. Detailed measurements of one sample confirm that these observations are due to a huge recuperation effect. The “shine plateaux” observed in the majority of these D_E determinations showed little increase of D_E with increasing exposure time. The mechanisms of this unexpected behaviour, and the implications for the detection of partial bleaching, are discussed.     

Changes in OSL properties of quartz by preheating: an interpretation

A study of OSL variation with preheat temperature showed, in a majority of cases, that OSL recorded at room temperature, increases above 200°C before the normal drainage at higher temperature. To explain this behaviour, an alternative interpretation to the common ‘electronic thermal transfer’ mechanism is suggested, supported by a study of hydrothermally grown quartz crystals. This interpretation involves impurities in substitution of Si⁴⁺, specially Al³⁺, which are associated with species like, in the case of quartz, hydrogen (H⁺, in fact, OH⁻) and alkali ions (Li⁺, Na⁺, K⁺). These monovalent ions usually act as charge compensators and are mobile during heating. As a consequence of the mobility and a possible irreversible exchange between compensators, the number of radiative recombination centres associated with the OSL trap(s), observable within the detection spectral window used (250–400 nm), increases during preheating. This phenomenon could lead to a wrong ED determination.     

Applicability of OSL pre-dose phenomenon of quartz in the estimation of equivalent dose

The feasibility of utilizing the pre-dosed OSL signal in the estimation of the equivalent dose has been investigated. The results based on (i) the behavior of growth curve, (ii) dose recovery tests and (iii) non-bleachability of reservoir centres, R-centres, suggests that (i) the pre-dosed OSL does not seem to work satisfactorily in dose estimation unlike the pre-dosed 110 °C TL emission and (ii) it may not be applicable in case of bleached specimen.     

Interlaboratory beta source calibration using TL and OSL on natural quartz

Laboratories using luminescence methods for dose reconstruction have to make interlaboratory source calibrations—initially this will be a single isotope beta or gamma source using one particular reference material. The procedure requires not only the administration of exact doses to the material but also the uniform handling of the dosimetric material and standardization of the procedures. An interlaboratory calibration of an Sr-90 beta source was recently carried out by our five laboratories which are involved in a retrospective project. The reference material was quartz but there were difficulties finding sufficient suitable quartz. Five different batches were obtained from the Merck company and tested for sensitivity, linearity and stability of the 340°C peak, the 1992 batch was found to be the most appropriate. The irradiations were performed at the Secondary Standard Dosimetry Laboratory at GSF using a Co-60 source as well as the in situ measurements with an ionization chamber, calibrated to the primary standards of PTB Braunschweig. Irradiated and unirradiated quartz was distributed to the five laboratories and although different procedures were used for thermoluminescence and optically stimulated luminescence, the source calibrations for the different laboratories agreed within ±3% compared to the previous calibrations of the laboratories.     

Component resolved OSL dose response and sensitization of various sedimentary quartz samples

The structure of the linearly modulated optically stimulated luminescence (LM-OSL) signal was studied for four sedimentary quartz samples, collected from different sites around Istanbul, Turkey. Applying a computerized deconvolution analysis to the LM-OSL curves, at least six individual components of first-order kinetics were identified and photoionization cross-section of each component was evaluated. The OSL dose–response curve of each component for each quartz sample was obtained, showing a remarkable differentiation from component to component. The behavior of a highly dosed sample to successive LM-OSL measurements was also studied showing a stable recuperation signal in the position of the “slow” and “medium” components and high resistance to OSL bleaching of the “slow” component. The individual sensitivity of each component as a function of the activation temperature was obtained. The sensitivity of each component was normalized over the respective sensitivity of the glow-peak at 110 °C of quartz in order to investigate the ability of the 110 °C glow-peak to act as a correction factor for all components of the LM-OSL curves examined.     

Influence of thermal treatment on OSL regeneration in potassium chloride

Optically stimulated luminescence (OSL) of pure analytical potassium chloride (KCl) prepared in two different forms (crystals and pellets) was studied. The occurrence of regeneration effect (self-renewal of the OSL signal) in the material was examined. The experiments using the variable delay OSL (VD-OSL) method were carried out. Performed measurements allowed to determine time scale of the phenomenon, as well as quantitative changes of regeneration depending on thermal treatment before and after irradiation. Significant increase of the OSL regeneration was noticeable for pellets after the application of the annealing before irradiation, while for crystals a substantial decrease of regeneration was observed. Preheating applied after irradiation caused that self-renewal of OSL signal was drastically reduced or completely suppressed depending on the form of KCl samples.     

Assessing the impact of pulsed-irradiation procedures on the thermally transferred OSL signal in quartz

Thermally transferred optically stimulated luminescence (TT-OSL) dating protocols have been suggested as a means of extending the age range of luminescence dating. Several studies demonstrate that TT-OSL signals increase with large radiation doses (>2000 Gy) and yet, few studies report older TT-OSL ages (>400 Gy) in agreement with independent absolute age control. In one such study, agreement with independent chronology was only achieved for the old samples by implementing a pulsed-irradiation procedure. Pulsed-irradiation is suggested to compensate for dose rate dependent competition effects by dividing the laboratory irradiation into discrete irradiation steps interspersed with heat treatments. However, every inter-step heat treatment has the potential to anneal part of the TT-OSL dating signal. This study compares constant- and pulsed-irradiation TT-OSL protocols and investigates the degree of partial thermal annealing. The results suggest that almost all of the difference in outcome between constant- and pulsed-irradiation protocols can be explained by partial annealing of the TT-OSL signal rather than by competition effects. Partial annealing distorts the laboratory dose response curve but has no impact on the natural signal, resulting in unreliable equivalent dose estimates. This means that pulsed-irradiation procedures may not be viable for TT-OSL dating measurements. Future studies implementing pulsed-irradiation procedures should carefully consider the extent to which inter-step thermal treatments partially anneal the signal.     

The dose dependency of the over-dispersion of quartz OSL single grain dose distributions

The use of single grain quartz OSL dating has become widespread over the past decade, particularly with application to samples likely to have been incompletely bleached before burial. By reducing the aliquot size to a single grain the probability of identifying the grain population most likely to have been well-bleached at deposition is maximised and thus the accuracy with which the equivalent dose can be determined is – at least in principle – improved.However, analysis of single grain dose distributions requires knowledge of the dispersion of the well-bleached part of the dose distribution. This can be estimated by measurement of a suitable analogue, e.g. a well-bleached aeolian sample, but this requires such an analogue to be available, and in addition the assumptions that the sample is in fact a) well-bleached, and b) has a similar dose rate heterogeneity to the fossil deposit. Finally, it is an implicit assumption in such analysis that any over-dispersion is not significantly dose dependent.In this study we have undertaken laboratory investigations of the dose dependency of over-dispersion using a well-bleached modern sample with an average measured dose of 36 ± 3 mGy. This sample was prepared as heated (750 °C for 1 h), bleached and untreated portions which were then given uniform gamma doses ranging from 100 mGy to 208 Gy. We show that for these samples the relative laboratory over-dispersion is not constant as a function of dose and that the over-dispersion is smaller in heated samples. We also show that the dim grains in the distributions have a greater over-dispersion than the bright grains, implying that insensitive samples will have greater values of over-dispersion than sensitive samples.     

OSL and IRSL characteristics of quartz and feldspar from southern California,USA

Southern California comprises of a wide range of diverse landscapes and environments, from high mountains with glacial and periglacial sediments to deserts with large sand dunes, extensive alluvial fans and ephemeral playas. Highly active tectonic processes has exposed ancient (c. 2 Ga) plutonic and metamorphic basement from deep within the crust, while similar Palaeozoic, Mesozoic and Cenozoic rocks are also common. A rich array of volcanic lithologies extending into the late Quaternary complement many thick sedimentary sequences that formed in equally diverse ancient environments typical of an accreting active continental margin. In some locations, notably in the Coachella Valley close to Palm Springs and the Salton Sea, low OSL sensitivity and poor characteristics restrict the application of the quartz SAR protocol to date late Pleistocene and Holocene fluvial sediments. In other locations such as the Malibu coastline, high sensitivity of the quartz OSL signal is observed, despite local source rocks being dominated by volcanic lithologies. Problems of poor quartz characteristics, along with uncertainty in predicting quartz OSL behavior for future dating campaigns poses a significant problem for projects, in particular for neotectonic contexts. While K-feldspar has been used extensively to date eolian and fluvial sediments in southern California, little information regarding signal stability is available. We explore the characteristics of both quartz and feldspar sub-samples from eolian, fluvial, lacustrine environments, in order to help develop mineral selection criteria for optical dating applications and clarify these issues. The importance of radiation quenching in quartz grains recently eroded from bedrock and the role of fires in enhancing OSL sensitivity are considered. The relative bleachability of quartz and feldspar fractions, along with thermal stability considerations is discussed. A simple test for quartz OSL signal contamination based on thermal quenching and assistance, and the susceptibility of the OSL signal to IR bleaching is introduced.     

Crushing effects on TL and OSL on quartz: relevance to fault dating

The effect of crushing on the TL and OSL signals in quartz was investigated to examine the feasibility of using OSL and TL for dating of faulted rocks. 275°C TL signals were not reduced by crushing by hand (mortar and pestle), in a pellet die press, or using an automatic mortar and pestle, but the sensitivity of the 100°C TL signal to a test dose decreased in crushed samples. Green light-stimulated OSL signal intensities were not decreased after crushing, but showed strongly increased inter-aliquot variability after crushing. We concluded that OSL and TL in quartz might be useful to characterize the crushing history of quartz in fault rocks, but their usefulness in dating fault events was not evident because we did not find evidence of signal zeroing under the conditions used in this study.     

Potential of the slow component of quartz OSL for age determination of sedimentary samples

The slow component of quartz OSL exhibits a high thermal stability, and, in many of the samples studied, a high dose saturation level (several hundreds or, even thousands, of Grays). These properties suggest that the slow component has potential as a long-range dating tool. Initial attempts have been made to obtain equivalent doses for a number of sedimentary samples. Single- and multiple-aliquot techniques were modified for use with the slow component. The results indicate that there is a good potential for sediment dating, particularly for samples of significant age. Experiments concerning the optical resetting of the slow component suggest that, given its slow optical depletion rate, dating may be restricted to aeolian sediments.     

Relative response of TL and component-resolved OSL to alpha and beta radiations in annealed sedimentary quartz

Knowledge of the relative luminescence response to alpha and beta radiation is very important in TL and OSL dating. In the present study the relative alpha to beta response is studied in a sedimentary quartz sample, previously fired at 900 °C for 1 h, in the dose region between 1 and 128 Gy, for both thermoluminescence (TL) and linearly modulated optically stimulated luminescence (LM – OSL). The LM – OSL measurements were performed at room temperature and at 125 °C. All OSL signals were deconvolved into their individual components. Comparison of OSL curves after alpha and beta irradiation strongly supports that quartz OSL components follow first order kinetics in both cases. In the case of TL, the relative alpha to beta response is found to be very different for each TL glow-peak, but it does not depend strongly on irradiation dose. In the case of LM – OSL measurements, it is found that the relative behaviour of the alpha to beta response is different for three distinct regions, namely the fast OSL component, the region of medium OSL component originating from the TL glow-peak at 110 °C when stimulation takes place at room temperature and finally the region of slow OSL component. Following stimulation at ambient temperature, the relative alpha to beta response of all components was not observed to depend significantly on dose, with the value of ratio being 0.03 and a tendency to decrease with increasing dose. However, in the case of measurements performed at 125 °C, the relative response of the fast components is much enhanced, and for the remaining components it increases with increasing dose. Special care must be taken to examine the relative alpha to beta response of the fast component at 125 °C which contrasts the relative response of the TL peak at ca. 325 °C. The implications for the dating of annealed quartz are also briefly discussed.     

Identifying well-bleached quartz using the different bleaching rates of quartz and feldspar luminescence signals

When dating older sedimentary deposits using quartz, there are no unambiguous methods for identifying the presence of incomplete bleaching. Current statistical analysis of dose distributions depends entirely on the assumption that incomplete bleaching and mixing are the main causes of any excess dispersion in the distribution; the only existing way to test this assumption is using independent age control. Here we suggest a new approach to this question, based on the differential bleaching rates of quartz and feldspar luminescence signals. We first present data that confirm the differences in relative bleaching rates of quartz optically stimulated luminescence (OSL) and feldspar luminescence stimulated at 50 °C by infrared light (IR₅₀) and feldspar luminescence stimulated at 290 °C by infrared light after a stimulation at 50 °C (pIRIR₂₉₀), and use recently deposited samples to determine the likely significance of the difficult-to-bleach residual feldspar signals in non-aeolian samples. For a set of mainly Late Pleistocene non-aeolian sediments, large aliquot quartz doses are then used to predict feldspar doses (based on a knowledge of the sample dose rates). The differences between observed and predicted feldspar doses as a function of the quartz dose, combined with a conservative assumption concerning the relative feldspar and quartz residual signals after natural bleaching prior to deposition, are used to identify those samples for which the quartz is very likely to be well bleached (20 out of 24). Two of these apparently well-bleached samples are then examined using single-grain quartz dose distributions; one of these is consistent with the well-bleached hypothesis, and one indicates poor bleaching or a multi-component mixture. However, independent age control makes it clear that the large aliquot data are more likely to be correct. We conclude that a comparison of quartz and feldspar doses provides a useful independent method for identifying well-bleached quartz samples, and that it is unwise to apply statistical models to dose distributions without clear evidence for the physical origins of the distributions.