Luminescence dating of volcanic eruptions in Datong,northern China

In this study, fine-grain quartz was used for luminescence dating for lava baked samples from different sites in Datong. Optical stimulated luminescence (OSL), thermal transferred OSL (TT-OSL)/recuperated OSL (Re-OSL) and thermoluminescence (TL) dating protocols were applied. For these samples, the OSL signals saturate at about 300–400 Gy, which limits their age to less than 100 ka based on their ambient dose rates. The TT-OSL/Re-OSL method has poor dose recovery. TL dating gives reliable results, and multiple-aliquot regenerative-dose TL method with sensitivity change correction based on the 325 °C TL peak of a test dose can be applied for samples up to 400 ka. The results indicate that the ages of the volcanoes in Datong are from 380 ka to 84 ka. The volcanic activity started earlier in the southeast area than those in the northwest part, which is consist with the literature data.     

Cosmogenic nuclide burial dating at Penhill Farm: An Earlier Stone Age Acheulean locality in the lower Sundays River Valley,South Africa

Penhill Farm is an Earlier Stone Age (ESA) Acheulean archaeological site located within the southeastern Cape coastal region of South Africa. Although ESA artifacts have been known for this region since the 1950s, limited archaeological work and an inability to date the terrace context sites have prevented understanding the technological progression from the ESA to Middle Stone Age (MSA) and their placement within the Stone Age chronology of South Africa. Here we use cosmogenic ²⁶Al and ¹⁰Be to reveal a two-stage depositional history for a stone tool assemblage recovered from a debris flow deposit, with artifacts dating to ca. 1.1 Ma (million years) incorporated into a debris flow dating to ca. 0.6 Ma, thereby constraining the Penhill Farm Acheulean occupation to the Early Pleistocene.     

Radiofluorescence of quartz: A review

Radiofluorescence (RF) is the luminescence emitted during exposure to ionizing radiation. Charged particles or high-energy photons can be used as stimulation sources, and different designs for measurement equipment have been published. Only few studies have successfully used the quartz RF signal for dosimetry and dating. However, RF is a valuable tool in deciphering charge trafficking in quartz crystals, and also provides information for identifying types of defects causing specific luminescence emissions. Based on models for charge transfer in quartz, RF is seen as resulting from direct recombination of electrons with holes captured in recombination centers (or vice versa) during ionizing irradiation. Competition between reservoir and luminescent centers explains the initial decay of the modeled RF curve followed by a steady rise and also the observed ‘pre-dose’ effect. Emission spectra have been found to be similar to thermoluminescence (TL) spectra, with prevalent emissions in the UV and further emissions for some samples in the blue-green and red range. The high intensity levels and the possibility of choosing longer accumulation times compared to TL and OSL are advantages of RF for spectral measurements. Relative peak intensities in the emission spectra change with dose and absolute intensities with dose rate. Investigating the RF signal with changing measurement temperature allows calculating physical parameters of individual emissions that control thermal quenching. The degree of thermal quenching varies between the emissions, with most intense quenching in the UV. Sensitization of RF by several orders of magnitude has been observed after annealing at 500 °C.     

Thermal behaviour of organic radicals and paramagnetic centres in chert: A case study of Bergeracois brown chert,Dordogne, France

In order to successfully understand the complex evolution of prehistoric societies, archaeologists require absolute dating tools, which are not only accurate but also widely applicable. Thermoluminescence (TL) dating is one such approach that has been successfully used to establish a general chronological framework for prehistoric sites and is particularly suited for use on heated lithic artefacts. Experiments conducted in this study have clearly shown the applicability of Electron Spin Resonance (ESR) isothermal modelling in combination with TL dating to constrain firing temperature. This expands the potential application for TL dating to include artefacts treated at low firing temperatures. The present study shows potential in terms of precision and accuracy for framing the “equivalent firing temperature”. At the same time, the comparison of the TL signal with the lattice-defects and aluminium centres invigorate the use of ESR dating on heated flint, especially with samples that have received low thermal treatment. The presence of organic matter in large quantity raises concern on the pyrolysis effect on the luminescence signal; however, the use of ESR isothermal and isochronal modelling could potentially lead to the ability to overcome current interferences of the organic radicals within the dating signal of TL.     

Electron spin resonance dating of quartz from archaeological sites at Victoria Falls,Zambia

When electron spin resonance (ESR) is applied to sedimentary quartz, dealing with the poor bleachability of the signals is particularly challenging. In this study, we used both the single-grain optically stimulated luminescence (OSL) and the single aliquot ESR dating of quartz from deep sand deposits preserving a Stone Age archaeological sequence to combine the advantages of the two methods: good bleaching behaviour and extended age range. Using the youngest samples at each sampling site we were able to calculate the mean ESR residual age from the difference between the OSL ages and the apparent ESR ages. Focusing mainly on the single aliquot regenerative dose (SAR) protocol here, we were able to calculate the mean ESR residual age for the Ti and Al centres, including the non-bleachable signal component for the latter. For the NP site, residual ages of 209 ± 13 ka and 695 ± 23 ka were calculated for the two centres, whereas for the ZS site 268 ± 39 ka and 742 ± 118 ka were determined. These residual ages are significant and cannot be neglected. Thus, the residual age was subtracted from the apparent ESR ages. The validity of the residual subtraction method was tested through a comparison of the oldest OSL age from each site with the residual subtracted ESR age. For both NP and ZS sites, the residual subtracted Ti and Al ages were consistent with the OSL age within 2-σ uncertainty, and therefore confirm the robustness of the subtraction method. Within the NP sequence, we were able to locate the end of the Early Stone Age at 590 ± 86 ka, and this provides a maximum age for the transition to the Middle Stone Age in this part of south-central Africa.     

石英热释光——沉积盆地热史研究中另一种潜在的古温标

具有良好重现性的石英热释光信号除了用于近地表的考古及地质事件定年以外,还能反映一定地质时间范围内的环境温度变化规律.本文利用砂岩中石英矿物的热释光信号,采用传统热释光分析和等温热释光方法,以东营凹陷中央背斜带钻孔岩芯为例,探讨对沉积盆地热体制信息的指示意义.研究表明：（1）钻孔中不同埋深位置的石英矿物,其自然热释光发光曲线有规律变化,与所对应的环境地层温度以及热释光发光动力学相符,即随着沉积地层埋深增加、埋藏温度上升与埋藏时间加大,其热释光发光曲线整体向高温方向移动,而发光强度明显减小;（2）石英热释光多片增加分析方法以及等温热释光分析方法所获得的表征年龄彼此印证,通过表征年龄的换算,定性或半定量获得描述沉积盆地热演化史的环境古温度变化的一个等效参数——表征温度,该表征温度能够表征沉积盆地一定地层范围内,一段埋藏历史的古温度变化历史.石英热释光信号是沉积盆地热史分析中一种潜在的古温标,对于石英热释光表征年龄与表征温度地质意义的诠释,仍需要更多的研究事例加以佐证.     

沂沭断裂带断层泥中 K-Ar、FT 和 TL 体系年代学含义的初步研究

本文报道了利用K-Ar法、TL法和FT法,分别测定断层泥中1Md伊利石(<1μ粒级组份)、石英(2-10μ粒级组份)和磷灰石单矿物的年龄结果;给出了沂沭断裂带三次强烈活动的年龄区间及强度逐渐减弱的变化趋势。首先提出了利用这三种测年手段,测定断层泥中三种不同物质的年龄,进而研究断层活动(强度和时间)的新方法     

Using R for TL dating

Whilst optically stimulated luminescence (OSL) is commonly more suitable for sediment dating because of faster signal resetting, thermoluminescence (TL) remains important for dating burnt material, e.g. in archaeological contexts, or for studying the luminescence properties of different materials. A lack of user-optimized analysis software for TL data has exacerbated the decline of TL dating in comparison to OSL. However, exciting developments in TL dating of flint and calcite indicate a rise in application of this underused method.R is a programming language and environment for statistical computing and graphics. It provides a wide variety of statistical and graphical techniques and is highly extendable. A package specifically designed for luminescence data analysis is available. However, it mainly includes functions for the analysis of OSL data. The TLdating package is a new R package specifically dedicated to TL dating. This package is designed to be fully compatible with the existing Luminescence package and is user-friendly. It includes functions for TL data pretreatment and palaeodose estimation using the MAAD and the SAR protocols. The functionality of the TLdating package is evaluated using heated flints from Taibeh, Jordan.     

Maximum age limitation in luminescence dating of Chinese loess using the multiple-aliquot MET-pIRIR signals from K-feldspar

Numerical dating of loess is important for Quaternary studies. Recent progress in post-infrared infrared-stimulated luminescence (pIRIR) signals from potassium-rich feldspar has allowed successful dating of Chinese loess beyond the conventional dating limit based on quartz optically stimulated luminescence (OSL) signals. In this study we tested the multiple-aliquot regenerative-dose (MAR) pre-dose multiple-elevated-temperature post-IR IRSL (pMET-pIRIR) procedure on samples from the palaeosol S5 (∼480 ka) and S8 (∼780 ka) layers from the Luochuan and Jingbian sections, respectively. The results show that (1) compared to sensitivity-corrected signal (L_x/T_x), a higher saturation dose is observed for the sensitivity-uncorrected MET-pIRIR signals (L_x), suggesting that MAR is advantageous for dating old samples; (2) negligible fading component can be achieved using the pMET-pIRIR procedure; (3) for the sample from the top of palaeosol S5, D_e values (1360 + 226/-167 Gy) broadly consistent with expected D_e (1550 ± 72 Gy) can be obtained using the sensitivity-uncorrected 300 °C MET-pIRIR signal. Our study suggests that a D_e value of about 1800 Gy may be the maximum dating limit of Chinese loess using the MAR pMET-pIRIR procedure.     

Optical dating of aeolian and fluvial sediments in north Tian Shan range,China: Luminescence characteristics and methodological aspects

Loess and fluvial sand are important materials for dating river terraces and alluvial fans. This study focuses on the methodological aspects of dating loess and fluvial deposits from the northern flank of the Tian Shan range, China, using sand-sized quartz and potassium (K) feldspar. Luminescence characteristics of quartz and K-feldspar were studied for searching suitable dating procedures. Our results indicate that 1) most quartz aliquots were contaminated by feldspar, and were dated using a post-infrared optically stimulated luminescence (post-IR OSL) procedure. A Fast ratio acceptance threshold of 15 can be applied to select these aliquots with post-IR OSL signals dominated by quartz OSL; 2) the multi-elevated-temperature post-IR IR stimulated luminescence (MET-pIRIR) procedures are applicable for K-feldspar. A test dose of ∼30% of the natural dose is appropriate for dating of older (>10 ka) samples. An Age (T, t) plateau test can be used to evaluate the dating results; 3) for the loess samples, both quartz and K-feldspar were well bleached and are suitable for dating. Dating using K-feldspar is preferred for its higher efficiency; 4) for the fluvial sand samples, only the quartz grains were fully bleached. Single-aliquot dating of quartz gives reliable ages.     

断层物质测年的热释光研究

断层物质ＴＬ测年的关键，是断裂运动产生的温压效应能否使断裂带内某些矿物原贮存的ＴＬ能量完全释放而“归零”。为此，进行了不同条件的高温、高压和位移速率变化等的模拟断裂运动的实验。结果表明，断裂运动产生的摩擦增温是使断层面上矿物ＴＬ强度减弱的主要因素。讨论了摩擦增温值与断裂运动时剪应力大小、断层泥厚度和断层位移间的关系，并得到了野外断层面上实际测试的证实。据此研究成果，还对小湾坝区Ｆ＿７断裂的活动时代进行了测定     

Luminescence from glacimarine sediment-trap samples at the Antarctic Peninsula

Radiocarbon (¹⁴C) dating yields variable and high reservoir and core-top ages for glacimarine sediments around Antarctica. To test the suitability of luminescence as an alternate dating method we investigated the effectiveness of clock zeroing (by daylight) within fine-silt-size siliciclastic sediments from year-long vertical-array sediment traps in Andvord Bay and Brialmont Cove at the Antarctic Peninsula. Both long-bleach and short-bleach multi-aliquot IR-PSL (infrared photon stimulated luminescence) and single-aliquot, post-IR blue-PSL dating tests were conducted. As well, dual-bandwidth-bleaching thermoluminescence (TL) tests were performed on samples from Brialmont Cove. These TL bleaching tests indicate that silt from the middle and bottom traps at this site has had little or no exposure to daylight, but that silt from the top trap has had some exposure. All 24 samples (representing different seasons and different trap depths) exhibit anomalously old apparent ages (12 ka–60 ka) across annual seasons and depths of deposition when either long-bleach multi-aliquot or late-background-subtraction single-aliquot PSL procedures were employed. Thus regional bottom silts would be unsuited for dating by these two luminescence dating approaches. However, a short-bleach multi-aliquot IR-PSL procedure yields the expected zero ages for several samples, a promising result that requires further exploration.     

Optically stimulated luminescence of amorphous/microcrystalline SiO2 (silex): Basic investigations and potential in archeological dosimetry

Unlike the well-studied optically stimulated luminescence (OSL) signal of (macrocrystalline) quartz, not much is known about OSL from natural amorphous and microcrystalline silicon dioxide. These materials – generally termed “silex” – were widely used for prehistoric tool production, and thermoluminescence (TL) is routinely applied do date the firing event of heated specimens. This study presents data on basic OSL characteristics of silex such as signal composition and component-resolved thermal stability as well as the applicability of OSL for dating of burnt lithic tools.Fitting of LM-OSL curves yielded similar components (mostly five) as observed for quartz, with the photoionization cross-sections being in the same order of magnitude for both materials. Three different methods (LM-OSL pulse annealing, short-shine pulse annealing as well as the varying heating rate method) were applied to study the thermal stability of components and allowed calculating trap parameters E and s, and hence the electron retention lifetime. Only the most light-sensitive (“fast-like”) component proved to be of sufficient thermal stability for dating applications, as evidenced from coherent experimental results. All other components already diminished at preheating temperatures > 200 °C. Pulse annealing measurements further indicate that electron populations sampled by OSL and those responsible for the ca. 380 °C TL-“dating peak” are not identical. Dose recovery tests applying an OSL-SAR protocol with “hot bleach” in between the regeneration cycles showed good reproducibility of a known dose if only the initial OSL signal (ca. 0–0.5 s at 90% LED power) is used. Finally, obtained OSL-SAR and TL ages based on the blue TL emission are in agreement within errors for two Middle Paleolithic archeological samples showing a “fast-like” component. These results verify the experimental findings of sufficient long-term stability of the initial OSL signal. Since not all silex specimens deliver a bright and stable OSL signal, optical ages of suitable samples may serve as an additional internal check for the paleodose estimate rather than substituting TL as a standard technique for dating of heated silex.     

北京延庆盆地50万年以来的主要构造事件及年代学的初步研究

延庆盆地是一个位于燕山山及脉南京的晚新生代形成的小型断陷盆地，通过对延庆盆地系统的野外调查，根据延庆分协的地貌，只物，断裂活动等特征，初步认为延就分协在过去约５０万年曾发生守三次对盆地地貌和沉积环境演化发生过重要升改变盆地演经过程的重大构造事件。     

Human activity during the late Pleistocene in the Lop Nur region,northwest China: Evidence from a buried stone artifact

The Lop Nur region, in the east part of Tarim Basin, was an important transportation junction between west and east, north and south Eurasia. However, previous studies on prehistoric human activity have concentrated mostly on the Bronze Age, whereas that during the Stone Age remains largely unresearched. Here, we present a new direct evidence of human activity in the late Pleistocene, recorded on a grinding stone buried in a lacustrine sediment section of the Lop Nur region. The grain size distribution of the sediment section indicates that the site was probably in the center of a lake with weak hydrodynamic environment. Therefore, the stone artifact can only be carried to here by people instead of river and it was never move as soon as left here. Results of radiocarbon dating, the evident stratigraphic relations between the stone artifact and the sedimentary formation, indicate that the human activity could extend to approximately 13 ka BP. Furthermore, the results of starch-grain and use-wear analyses suggest that ancient humans gathered seeds of Triticeae, roots, and tubers and used the grinding stone to simply process selected plant as plant foodstuffs during this period. It implies that the environmental conditions in the river delta of the Lop Nur were inhabitable during the late Pleistocene.     

Validating post IR-IRSL dating on K-feldspars through comparison with quartz OSL ages

Recent developments have opened up the possibilities of using potassium feldspar for dating Pleistocene sediments; a stable (less-fading) part of the infrared stimulated luminescence (IRSL) signal can be selected by largely depleting the unstable part of the IR signal, using a combination of thermal and IR stimulation: post IR-IRSL dating (pIR-IRSL).This study aims to test the validity of pIR-IRSL dating on feldspars. We obtained pIR-IRSL ages on a large suite of samples from several locations in the Netherlands area, covering a wide range of depositional environments and ages. Age control was provided by quartz optically stimulated luminescence (OSL) ages on the same samples; these ages were shown to accord with geological age constraints. Comparison with IRSL ages enabled us to evaluate the improvement that pIR-IRSL dating provides over conventional IRSL methods.The majority of feldspar ages obtained with pIR-IRSL showed good agreement with both the quartz OSL ages and the geological age constraints. Our study demonstrates that pIR-IRSL dating is more robust than conventional IRSL and should be the method of choice in feldspar luminescence dating of Pleistocene sediments.     

Luminescence determination of firing temperature of archaeological pure sand related to ancient Dian bronze casting,China

In the present paper, we have investigated the thermal history of an archaeological ‘core sand’ from a cow-shaped bronze ornament attached to a cowrie container. It was unearthed at the Lijiashan site, located in southwest China, in the area of central Yunnan, and dates from the Han period (3 c. BC–2 c. AD). We compared the archaeological sample and a control sample of the modern quartz, examining the sensitivity of 110 °C TL and 210° C TL glow peaks, and sensitization characteristics of 110° C TL and OSL. Large differences between the ‘core sand’ samples and the control sand samples have been observed in our work. The firing temperature of the ‘core sand’ was determined to be 550–700 °C. The results offer a key to understanding the ‘core sand’ as a unique casting technique in Bronze Age Yunnan. These luminesence techniques form a new method for determining the historical firing temperature of archaeological material.     

Residual thermoluminescence for sun-bleached quartz: Dependence on pre-exposure radiation dose

Quartz grains zeroed by heat and subsequently irradiated—either in the laboratory, or naturally in volcanic deposits—were exposed to sunlight for several months prior to TL measurements. As a result, the residual TL, in either the Blue or the Red, appeared to grow significantly with the radiation-dose experienced by the grains since zeroing. In another experiment, unheated sedimentary quartz grains, sampled at the very surface of a coastal sand-dune, were irradiated and subsequently exposed to sunlight before TL measurements. The residual Red-TL still exhibited a strong dose-dependence, but at a level that was higher than the natural signal. Finally, it was concluded that the so-called “unbleachable TL” is not a constant, intrinsic quantity, for a given quartz sample.

Because the residual TL is strongly correlated with the radiation dose experienced since the last zeroing by heat, it can theoretically be quoted in terms of “dose”, as is sometimes done. However, this raises the question of its correct evaluation, and, on the other hand, there is a risk of misinterpreting its physical meaning in the case of unheated sediments.

In the context of sediment dating, the experimentally-estimated residual signal that is routinely subtracted from the total signal for palaeodose estimation is, therefore, higher than the signal that would have been measured prior to burial. Such an effect introduces an error that can be significant for Red TL. It can be corrected for, at least approximately, from experimental exploration of the dose-dependence of the residual TL.     

Investigating the effect of diagenesis on ESR dating of Middle Stone Age tooth samples from the open-air site of Lovedale,Free State,South Africa

Teeth are usually targeted for dating archaeological sites because they are less prone to dissolution, in comparison with bones. However, despite this apparent resistance, teeth do undergo diagenesis, which needs to be accounted for in order to obtain accurate ages. In particular, the uptake of trace elements such as uranium in dental tissues needs to be considered for dose rate determination when dated using electron spin resonance (ESR). Characterising the mineralogy and structural integrity of samples prior to dating may thus provide important information related to their state of preservation, especially in the case of teeth whose U content can significantly affect the dose rate.In this study, we dated five teeth of small-sized bovids using combined ESR/U-series dating. They were collected at the Middle Stone Age site of Lovedale, located in the central interior of South Africa. Micromorphology provided sedimentary context to the samples, which were recovered from a layer of gravel rich in faunal remains. Using cathodoluminescence, laser-induced fluorescence, Fourier transform infrared spectroscopy and Raman micro-spectroscopy we assessed the degree of preservation of the enamel. Results reveal that carbonate hydroxyapatite underwent post-depositional alteration, based on its molecular structure and elemental composition. Although the teeth all originate from the same layer and were sampled in the same 1-m square and at a similar elevation, U-content in the enamel differs highly from one tooth to the other, with values ranging from 1.7 to 29.6 ppm. These values are correlated with equivalent doses (D_e) from 228 to 923 Gy and are consistent with variations in crystallinity determined with vibrational spectroscopy. We also investigated the possible saturation of the ESR signal, by repeating measurements with microwave power values from 1 to 20 mW.Despite such diversity in U-content, the ages calculated assuming an early uptake of U all fall within the same range, from 63 ± 8 ka to 68 ± 15 ka and may only represent a minimum estimate.     

Extending the age limit of luminescence dating using the dose-dependent sensitivity of MET-pIRIR signals from K-feldspar

We investigated the sensitivity change of multiple-elevated-temperature (MET) stimulated post-infrared infrared-stimulated luminescence (MET-pIRIR) signals as a response to irradiation, sunlight bleaching and heating using samples from the Mu Us Desert, central China. A strong dose dependence of MET-pIRIR signal sensitivity was observed. The intensity of the test-dose signals (T_x) increase with the pre-dose received. Furthermore, the signal sensitivity can be reset by sunlight bleaching or heating. This suggests that both the electron traps and hole centres in K-feldspar can be bleached by sunlight, and can, therefore, be used for dating. Using the test-dose signal as a monitor for sensitivity change, it was found that the sensitivity (or hole centres) saturate at a higher dose (D₀ = ∼750 Gy) than the sensitivity-corrected signals (or electron traps) (D₀ = ∼400 Gy). We propose a multi-aliquot regenerative-dose (MAR) MET-pIRIR dating protocol, which utilises the high saturation dose of hole centres. This protocol was tested using aeolian sediments from north China with ages ranging from 0 to 470 ka. It was found that, compared to the dose limit of ∼800–1000 Gy using the normal MET-pIRIR or pIRIR procedure, the new method can measure a natural dose of up to ∼1500 Gy and produce ages consistent with the expected ages for the samples investigated.