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.     

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.     

Study of the 110°C TL peak sensitivity in optical dating of quartz

As the 110°C TL emission in quartz uses the same luminescence centers as the OSL emission, the 110°C TL signal from a test dose may be used to monitor the OSL sensitivity change. It is thus important to study the relationship between the 110°C TL peak and the OSL sensitivity in studies related to optical dating from quartz. We have conducted a series of experiments using sedimentary quartz, where the annealing temperatures were varied between 260 and 1000°C before the measurement of OSL and 110°C TL sensitivities. Another series of experiments on two sedimentary quartz samples investigated the 110°C TL peak and OSL dose-dependent sensitivity change after different annealing temperatures. In these experiments, the 110°C TL and OSL signals from the test dose are shown to have similar sensitization characteristics: the 110°C TL sensitivity change is proportional to the OSL sensitivity change if the annealing temperature is lower than 500°C. It is concluded that the 110°C TL signal can be used to correct the OSL sensitivity change in the single-aliquot additive-dose protocol.     

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.     

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.     

Luminescence sensitivity changes in quartz as a result of annealing

Retrospective dosimetry using optically stimulated luminescence (OSL) on quartz extracted from (for example) bricks needs to account for strong OSL sensitivity changes that are known to occur depending on the previous thermal treatment of the sample. Non-heated quartz exhibits OSL orders of magnitude less per unit radiation than that for heated material. The reason these temperature-induced sensitivity changes occur in quartz is presently not well understood. This phenomenon is also seen in the related area of luminescence dating in which sedimentary quartz and quartz from heated archaeological samples show very different OSL sensitivities. In this paper we report on studies of the effects of high temperature annealing on the OSL and phototransferred TL (PTTL) signals from sedimentary and synthetic quartz. A dramatic enhancement of both OSL and PTTL sensitivity was found especially in the temperature range 500–800°C. Computer simulations of the possible effects are shown to produce data that agree in all essential details with the experimental observations. It is further demonstrated that the enhanced OSL sensitivity as a function of annealing temperature is not a pre-dose effect.     

Kinetics of red, blue and UV thermoluminescence and optically-stimulated luminescence from quartz

The duration over which charge is retained at trapping sites is of fundamental importance for trapped electron dating. Here, we report measurements of the kinetic parameters of the prominent thermoluminescence (TL) glow peaks of quartz, and of the optically-stimulated luminescence (OSL) signal from quartz utilised for optical dating. The similarity in trapping lifetimes of the 325°C TL peak and the dominant component of the OSL signal are taken as further support for the hypothesis of their common origin in the same trapped electron population.     

Comparison of the properties of various optically stimulated luminescence signals from potassium feldspar

Various optically stimulated luminescence signals from K-feldspar have been used to determine the equivalent doses of sediment samples. Understanding the properties of these optical signals is critical to evaluate their applicability and limitations to optical dating. In this paper, some properties of IRSL, post-IR OSL and post-IR IRSL signals (detected in the UV region using U-340 filters) from a museum sample of K-feldspar were investigated by analyzing the relationships between optical and TL signals, and the effect of optical bleaching and heating on optical signals. The trap parameters of the different optical signals were calculated using the pulse annealing method. The results show that this sample exhibits two regenerated TL peaks at ～140 and ～330 °C. Corresponding to the low temperature TL peak, the OSL and post-IR OSL signals appear to be more associated with lower temperature TL than the IRSL signal measured at 50 °C. Corresponding to the high temperature TL peak, the post-IR IRSL signals mainly originate from the more thermally stable traps associated with the high temperature TL, compared with the IRSL and post-IR OSL signals. However, the post-IR IRSL_225 °C signal is shown to be hard to be bleached by blue light and simulated sunlight, compared with the IRSL_50 °C and low temperature post-IR IRSL signals. The implication for optical dating is that the elevated temperature post-IR IRSL signals can be preferentially applied over other signals from K-feldspar, but it is desirable that the effectiveness of the pre-depositional zeroing of these signals is assessed.     

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.     

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.     

Observations of thermal transfer OSL signals in glacigenic quartz

The conclusions of Rhodes and Pownall (Rhodes, E.J., Pownall, L., 1994. Zeroing of the OSL signal in quartz from young glaciofluvial sediments. Radiation Measurements 23, 329–333) were somewhat discouraging for the prospects of using quartz OSL for dating glacigenic sediments, while the more detailed study of Rhodes and Bailey (Rhodes, E.J., Bailey, R.M., 1997. The effect of thermal transfer on the zeroing of the luminescence of quartz from recent glaciofluvial sediments. Quaternary Science Reviews (Quaternary Geochronology) 16, 291–298) provided more encouragement. Specifically, the latter authors were able to account for the relatively high D_e values observed for recent glacigenic (dominantly glaciofluvial) sediments in terms of an anomalously high thermal transfer effect, rather than simply insufficient bleaching prior to deposition. In other locations, the OSL of quartz from glacigenic material appears to provide reliable age estimates, and does not suffer from these effects (Owen, L.A., Richards, B., Rhodes, E.J., Cunningham, W.D., Windley, B.F., Badamgarav, J., Dorjnamjaa, D., 1998. Relic permofrost structures in the Gobi of Mongolia: age and significance. Journal of Quaternary Science 13 (16), 539–548; Richards, B.W., Owen, L.A., Rhodes, E.J., 2000. Timing of Late Quaternary glaciations in the Himalayas of northern Pakistan. Journal of Quaternary Science 15, 283–297). In this paper, laboratory bleached samples from both the above studies are remeasured, using an experimental design to correct for OSL sensitivity changes, which has some similarities to the single aliquot regenerative dose (SAR) protocol of Murray and Wintle (Murray A.S., Wintle A.G., 2000. Luminescence dating of quartz using an improved single-aliquot regenerative-dose protocol. Radiation Measurements 32, 57–73). Clear evidence of thermal transfer OSL signals, generated during the preheating procedure, is presented. Further measurements, using the full SAR protocol, demonstrate that the source of this charge is related to natural dosing. For one sample, the apparent effect is subtracted effectively by the SAR protocol. Another sample studied in detail shows a striking relationship between the thermally transferred OSL signal and the total TL observed during the ramping of the preceding preheat treatment.     

Sediment dating by luminescence: a review

In the present article we review applications of luminescence methods for the determination of the age of sediments for Quaternary Earth science. “Sediment” is taken to include any mineral particles transported by wind, water and/or ice and subsequently deposited. Methodology is not discussed per se but appears in context. The emphasis is on recent work and is illustrative rather than exhaustive. Applications in archaeology are mentioned only briefly. Successful dating requires that the luminescence signal has been zeroed by sunlight at the time the sediment was laid down. Dune sands and loess transported in full daylight usually satisfy this condition and have been dated by both traditional thermoluminescence and by optical methods. Optical dating is advantageous for less well-bleached sediments, such as are found in colder climates and those laid down by fluvial and glacial processes, although the prospects for dating the latter are shown to be poor. Among less common contexts are volcanic eruptions, earthquake faults and tsunami deposits. The dating of very young sediments, less than 2 ka, is demonstrated and the factors limiting the dating of very old sediments, 500 ka to 1 Ma, are discussed. Validation of any dating method by comparison with other methods is necessary; luminescence ages have been successfully compared with ages obtained by, for example, ¹⁴C, U–Th series and δ¹⁸O isotope ratios. The most difficult problems encountered in dating quartz, feldspars and undifferentiated fine grain mixtures include: anomalous fading (which leads to underestimates of age), incomplete zeroing (which gives overestimates) and sample inhomogeneity. Methods devised to minimise these effects include preheating regimes, selection of observing wavelengths and of stimulating wavelengths for optical dating, the use of single aliquot and single grain measurements. The use of appropriate data analysis procedures is also important. Advice on current best practice on procedures for obtaining reliable ages is offered and, in all applications, there are suggestions as to where further research might be directed.     

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.     

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.     

First steps toward spatially resolved OSL dating with electron multiplying charge-coupled devices (EMCCDs): System design and image analysis

Spatially resolved OSL (SR-OSL) measurements are made with a scanning or imaging system that records luminescence emissions from known sources within a sample. This work is a first step toward the development of an SR-OSL methodology based on the imaging of ultraviolet OSL emissions with an EMCCD camera. We present UV OSL images of natural quartz extracts, OSL/TL/IR images of sandstone, image-based OSL measurements from aluminum oxide grains, and dose recovery experiments on aluminum oxide and Risø calibration quartz. Camera sensitivity and quantitative reproducibility indicate that EMCCD-based OSL dating is feasible. Further experimentation is necessary to adequately define the error sources and measurement limitations of EMCCDs in the OSL regime.     

Lumineszenzdatierung quartärer Sedimente

The purpose of this paper is to discuss briefly the basis, technique and efficiency of luminescence dating. Thermoluminescence and optically-stimulated luminescence are useful for dating of quaternary sediments. Contents: Sediment Dating, Thermoluminescence Dating, Thermoluminescence (TL), Dating Method, Sources of Error, Dosimetry, Dating Techniques, Optical Dating (OSL), Sediments, References.     

LiMgPO_4:Tm,Tb的热释光和光释光陷阱参数

采用高温固相法合成了LiMgPO_4:Tm,Tb粉末样品,测定了热释光陷阱参数激发能E和频率因子s.用脉冲退火和多次退火方法研究了其光释光陷阱参数E和s,并与用多速法得到的热释光的结果进行了比较.对不同β射线剂量照射的样品发光曲线的研究表明,300°C高温峰属于一级动力学发光峰.通过对热释光和光释光陷阱的相关性研究表明,经200°C预热的热释光信号(对应于300°C高温峰)和光释光信号很有可能来自于同一深度的陷阱.     

Improving the TT-OSL SAR protocol through source trap characterisation

Thermally-transferred optically stimulated luminescence (TT-OSL) extends the age range of OSL dating using quartz. A set of experiments have been undertaken to determine the kinetic parameters of the TT-OSL source traps, and this information has been used to propose an improved TT-OSL single aliquot regenerative (SAR) dose protocol. By combining together OSL and thermoluminescence (TL) measurements on fine-grained quartz, a correspondence between TL peaks and the TT-OSL signal is found. The thermal stability of the main TT-OSL trap was estimated by applying Hoogenstraaten’s method and allowing for thermal quenching; this predicts a lifetime of 4.5 Ma at 10 °C. A set of experiments were undertaken to refine the treatment needed at the end of each SAR cycle to erase the previously acquired TT-OSL signal. An improved TT-OSL SAR protocol using this treatment is proposed, and it is tested on quartz from a young Holocene sample. These tests yielded excellent recycling ratios and excellent dose recovery.     

A practical correction for sensitivity change in thermoluminescence multi-aliquot-regeneration dating of feldspar dominated fine grain loess

Multi-aliquot (MA) thermoluminescence (TL) has been used little since the advent of modern single-aliquot-regenerative-dose (SAR) sediment dating methods for both quartz and feldspar. However, for dating unheated feldspar-bearing sediments older than 100–200 ka, MA TL can still be useful. To improve precision in burial-dose estimation from TL, a post-bleaching regenerative-dose procedure is beneficial. However, the long-known regenerative-dose TL sensitivity changes cause significant age under-estimation in such MA TL. Here a practical procedure is demonstrated to correct for this post-bleaching sensitivity change. Two samples of fine grain, polymineral loess having independent ages of ∼130 ka and ∼350 ka are employed with the use of the SLIDE (combined additive-dose and regenerative-dose responses) procedure to show that not only accuracy but improved precision can be attained with use of this practical procedure. The procedure employs an operational definition of laboratory-dose sensitivity change with respect to a second-glow TL signal, and corrects for the sensitivity change as a function of laboratory dose and of glowcurve temperature.