Thermal characterization of ancient hearths from the cave of Les Fraux (Dordogne,France) by thermoluminescence and magnetic susceptibility measurements

Numerous sorts of evidence of fires were observed in the cave of Les Fraux (Dordogne, France) and in particular the effects of fire on sediment were studied for a better understanding of their use centuries ago. Our present objective is the evaluation of the firing intensity by determining the past temperature (paleotemperature) attained by the topmost sediment of the archaeological fires. The principle of paleotemperature determination is based on the thermoluminescence (TL) properties of quartz and the magnetic susceptibility of the sediment. By comparing the TL signal of anciently heated quartz to the TL signal of thermal references made in the laboratory, we were able to obtain a maximal equivalent temperature attained for each sample extracted from ancient fires. The magnetic susceptibility (previously measured on the hearth surface) could thus be estimated as a function of temperature. The main result of this study is the temperature mapping of the hearth which can be used as meaningful information about the ancient firing intensity.     

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.     

用电子自旋共振（ESR）测年法测定断层活动年代的探讨

阐述了断层泥石英颗粒ＥＳＲ信号达到零化的温度和压力环境，通过４个具体ＥＳＲ测年实例，论述了测年样品的不同零化程度和测年数据的可靠性。对ＥＳＲ信号与ＴＬ（热释光）信号零化环境的差别及其原因进行了初步的探讨。介绍了断层测年样品ＥＳＲ信号达到零化的验证的方法。同时，提出了断层测年样品采集时应注意的有关问题     

ESR dating in Song Terus cave (East Java, Indonesia)

Electron spin resonance (ESR) dating on teeth has been used to determine the antiquity of the human presence in the area of Gunung Sewu (East Java, Indonesia). The Song Terus cave is one of the archaeological sites located in this area, which has yielded an important collection of fossil bones and prehistoric lithic industry. ESR dating shows that this cave belongs to a karstic system which has been in place since Middle Pleistocene. The results of coupled ESR/Uranium-series dating indicates closed system for uranium in tooth tissues yielding ages of between 216 and 392 ka for the oldest archaeological levels, confirming the possibility of finding Middle Pleistocene human occupations in such karstic sites in Java.     

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.     

Testing the application of post IR IRSL dating to Iron- and Viking-age ceramics and heated stones from Denmark

In this study we test, for the first time, the potential of an elevated temperature post-IR IR (pIRIR₂₉₀) SAR protocol for the dating of young heated artefacts. Seven heated stones and seven potshards were collected from three different archaeological sites in Denmark: one site from the early Pre-Roman Iron Age 200 BC to AD 100, and two from the Viking period between AD 800 and 1200.We first derive quartz OSL ages for these samples, to support the archaeological age control. The luminescence characteristics of the pIRIR₂₉₀ signal are then investigated; in particular the dose recovery ratios are shown to be close to unity. The performance of the feldspar pIRIR₂₉₀ protocol is then examined by comparing the pIRIR₂₉₀ ages with those based on the quartz OSL signal; the average ratio of pIRIR₂₉₀ to OSL ages is 1.14 ± 0.05 (n = 14) and there is some suggestion that the possible overestimation of the feldspar ages compared to quartz is only of significance for the heated stone samples. Nevertheless, there is no indication of incomplete heating of the stones; the ratios of D_e derived from the IR₅₀ and pIRIR₂₉₀ signals are independent of sample type, and consistent with complete resetting by heating. Comparison with the archaeological age control is not able to identify whether quartz or feldspar provides the most reliable dating signal.     

断层粘滑摩擦增温的理论分析及其对TL,ESR测龄的意义

采用断层位错模式,考虑了具有一定宽度的断层在其粘滑过程中,断层摩擦应力和滑动速度随粘滑过程的变化情况,由此计算了粘滑所产生的摩擦增温,并将结果与不考虑摩擦应力变化、不考虑滑动速度变化或忽略断层宽度时的情况作了比较。结果表明:断层滑动时,摩擦应力和滑动速度随时间的改变及断层的宽度将对断层摩擦增温产生较大影响。由于岩石中孔隙和孔隙流体的存在,摩擦应力在断层粘滑过程中有较大变化。取断层滑动速度为Brune 震源时间函数形式,考虑摩擦应力的变化及一定的断层宽度,计算得到的摩擦增温值较以往的计算结果偏小。这个结论对测定断层活动年代的热释光(TL)和电子自旋共振(ESR) 法具有一定的理论指导意义     

ESR dating of glacial moraine deposits: Some insights about the resetting of the germanium (Ge) signal measured in quartz

The electron spin resonance (ESR) dating of tills using germanium-doped (Ge) paramagnetic centers in quartz has advantages over other dating techniques, as quartz is common, processing is easy, and the technique has the potential for dating features several hundreds of thousands years old. ESR dating of moraines is based on the supposition that either subglacial comminution or exposure to sunlight resets the signal. However, actual dating suggests that a signal that is initially present cannot be bleached to zero by grinding alone. We found that grinding coarse samples (0.5–1 mm in diameter) to the mean grain size of fine sand (0.125–0.193 mm) reduced the signal intensity to 53–69% of its original value. From the value of the signal difference, one can devise a correction factor for ESR ages of subglacial sediment. Polymineralic grains are commonly present in till. Exposure of them to sunlight for several days can reduce the signal intensity to 7–8% of its original value within 1–2 mm thick of the sediment surface. However, within 5–8 mm of the sediment surface, exposure to sunlight for over one week only reduced the signal intensity to mean plateau values of 42–50% of the initial value. Mixing upper and lower layers of the samples during exposure to sunlight changed the signal intensity. This suggests that the amount of bleaching varies spatially. Sediments initially deposited at the margins of ice caps or ice sheets and subsequently overridden may have been sufficiently exposed to sunlight to allow ESR dating of moraines. The purity of the quartz and the grain size have significant impacts on signal intensity; intensive purification and the use of a uniform fine sand fraction are thus recommended.     

Preliminary ESR dating results on loess samples from the loess–paleosol sequence at Luochuan, Central Loess Plateau, China

The quartz Al centre has been used in pioneering studies for ESR dating of sediments. Acceptable age estimates could be obtained for a range of deposits using this centre after estimating the residual level. To inspect the feasibility and reliability of ESR dating of windblown sediments, six loess samples from the loess–paleosol sequences of Luochuan profile on central Loess Plateau, China, were dated by ESR with regeneration method using the quartz Al centre measured at 115 K. The samples were exposed to sunlight for 430 h. Only about 25% signal intensity was bleached. According to our preliminary results, ESR age estimates increased with the depth along the loess profile, however, the ESR age of each sample is only about a half of the reference age of the corresponding strata. For example, the ESR age of a sample from the top of L₈ loess near B/M boundary (a known age of 780 ka) yields an age of only 385 ka. It seems that ESR dating using quartz Al centre with dose regeneration protocol may have the potential for dating of loess and other aeolian deposits, but the studies on the nature of the quartz Al centre and experiment protocols have to be studied further.     

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.     

ESR and OSL dating of fossil-bearing deposits from Naracoorte Cave Complex palaeontological sites,south Australia

Little work has been undertaken on combined dating of sedimentary quartz grains using electron spin resonance (ESR) and optically stimulated luminescence (OSL) techniques in Australia. This study aims to assess the suitability of a combined ESR and OSL dating approach for establishing improved chronologies of Middle-Late Pleistocene deposits within the Naracoorte Cave Complex (NCC), South Australia. Here, we apply ESR and OSL dating in tandem to a series of samples collected from three different NCC sites: Whale Bone, Specimen and Alexandra cave. ESR quartz dating focuses on the multi-centre (MC) approach, which involves comparative evaluations of Al and Ti centre signals, while paired luminescence dating focuses on single-grain OSL analysis and includes examination of multi-grain averaging effects. The comparative ESR-OSL dating results exhibit broad agreement for deposits spanning 50–150 thousand years, with either the Ti–H or Al centre ages overlapping with paired OSL ages at 2σ in nearly all cases. MC ESR evaluations (Al v Ti–Li v Ti–H age assessments) indicate incomplete resetting of the bleachable Al centre signal for a small number of samples. Two-thirds of samples exhibit Ti–Li ages that are significantly older than corresponding Al centre ages, which is unexpected from a bleaching kinetics perspective and may indicate a broader reliability issue for Ti–Li palaeodose evaluation with these particular samples. Our findings: (i) support the applicability of both palaeodosimetric dating methods in this depositional setting; (ii) highlight the merits of applying combined ESR-OSL analyses in tandem, and; (iii) provide one of the first reliable evaluations of quartz ESR MC dating for samples with natural dose ranges as low as only a few tens of Gy. These results show that the Whale Bone, Specimen and Alexandra cave sites are temporally related and can be used to derive multi-site reconstructions of faunal assemblages and palaeoenvironmental history.     

ESR dating of the Eupchon fault, South Korea

We investigated temporal pattern of Quaternary fault activity of the Eupchon fault zone in the southeastern part of the Korean peninsula, using ESR dating of fault rocks. The counterfeit E′ signal significantly affected the equivalent dose on some samples. In particular, the counterfeit E′ signal tends to affect samples with E′ intensity close to saturation level. Storage at room temperature for 360 days and heating at 170 °C for 15 min. after γ-ray irradiation did not change significantly the intensities, the dose responses and ESR ages for OHC, Al, and Ti signals. ESR ages from the Eupchon fault zone range from 2000 to 500 ka. The fault rocks were reactivated at least five times 2000, 1300, 900–1100, 700–800, and 500–600 ka ago. These data indicate that long-term cyclic fault activity of this fault zone continued into the Quaternary. The results from this study suggest that the Eupchon fault zone can be classified as a potentially active fault and presents some potential seismic hazards to the nuclear power plant in its vicinity.     

Optical dating of perennially frozen deposits associated with preserved ancient plant and animal DNA in north-central Siberia

We present chronological constraints on a suite of permanently frozen fluvial deposits which contain ancient DNA (aDNA) from the Taimyr Peninsula of north-central Siberia. The luminescence phenomenology of these samples is first discussed, focusing on the optically stimulated luminescence (OSL) decay curve characteristics, thermoluminescence (TL) properties, and signal compositions of quartz from these previously unstudied deposits. Secondly, we assess the suitability of these samples for OSL dating and present the OSL chronologies obtained using both single-grain and multi-grain equivalent dose (D_e) measurements. The results of our analyses reveal a large amount of inter-aliquot variability in OSL decay curve shape that is directly related to differences in the size of the 280 °C TL peak and the associated slowly bleached ‘S2’ OSL component. Longer OSL stimulation durations are adopted in the D_e measurement procedure to prevent the progressive build-up of slowly bleached signal components throughout successive single-aliquot regenerative-dose (SAR) measurement cycles. The use of low preheat temperatures in the SAR procedure also reduces the deleterious effects of these slowly bleached signal components. The resultant single-grain and multi-grain OSL chronologies obtained using this approach are stratigraphically consistent and are in close agreement with independently established ¹⁴C ages at our sites. The findings of this research reveal the potential of OSL dating as a means of providing a reliable chronometric framework for sedimentary aDNA records in permafrost environments.     

The application of two‐dimensional hydrodynamic models for underwater archaeological finds from the Vistula River in Warsaw,Poland

Low water levels occurring on the Warsaw section of the Vistula River during droughts in 2012 and 2015 stirred considerable interest by exposing parts of the riverbed. The river's low flow discharge created favourable conditions for archaeologists who, from the river's bottom, managed to salvage sculptures, architectural artefacts, and military accessories dating back to the middle of the 17th century. Literature shows that archaeological finds at the bottom of a major lowland river are unique and are attributed to very specific hydrological and geological conditions. Embankments and works meant to regulate the channel of the Vistula River in Warsaw narrowed the channel and accelerated the erosion of the river's bottom. A comparison of rating curves created between 1919 and 2015 shows that the river's bottom had lowered by 225 cm. The diameter of sediment particles that could be moved at maximum shear stress has been calculated using the Meyer–Peter and Muller formula. According to the calculated shear stress corresponding to the highest historical flood of 1844 particles smaller than 0.05 m were transported down the river, and it is true that artefacts of that size had not been collected at the site. Taking into consideration the very specific geological and hydrological conditions, we believe that finding so many 17th century artefacts with a well‐documented history at a site at the bottom of major lowland river with intensive channel processes is indeed unique. Additionally, it is the first time that results of hydrodynamic modelling have been successfully used for archaeological survey to define the critical shear stress and the smallest diameter of artefacts, which could remain stable on a river's bottom.     

ESR and ESR/U-series dating study of several middle Palaeolithic sites of Pléneuf-Val-André (Brittany,France): Piégu,Les Vallées and Nantois

The area of Pléneuf-Val-André, Brittany, France, has delivered several Palaeolithic sites containing palaeontological remains, very rare into this granitic area. In order to precise the stratigraphical framework of the prehistoric human occupations of this zone, an ESR dating program was initiated in the late 1980s and different kinds of materials (mammal bones and teeth, naturally bleached quartz extracted from marine or aeolian sediments and marine mollusc shells) were then sampled for geochronological analyses. The present paper displays the main obtained results on three stratigraphically connected middle Palaeolithic sites: Piégu, Les Vallées and Nantois. The results are consistent with the regional chronostratigraphic framework and permit to suggest palaeoenvironmental reconstruction of the area and the dating of the various archaeological evidences.     

ESR dating of optically bleached quartz grains from Plio-Pleistocene to Holocene coastal dune deposits (Wilderness-Knysna area,South Africa): a comparison with luminescence

Five Plio-Pleistocene to Holocene aeolian quartz samples from the coastal dune deposits of the Wilderness-Knysna area (South Africa) previously dated by OSL were selected for ESR dating. Samples were processed following the Multiple Centre approach and using the Multiple Aliquot Additive dose method. Aluminium (Al) and Titanium (Ti) signals were systematically measured in all samples.Our study shows that ESR results obtained for Middle Pleistocene to Holocene samples may be strongly impacted by (i) the presence of a significant high frequency noise in the ESR spectra acquired for the Ti signals and (ii) the choice of the fitting function employed. In particular, if not taken into account, very noisy spectra can lead to a significant overestimation of the true ESR intensity measured for the Ti–H signal. These sources of uncertainty are however not sufficient to remove the ESR age overestimations. Consequently, our results indicate that the Al and Ti ESR signals of these quartz samples have not been fully reset during their aeolian transport.While this work contributes to improve our understanding of the ESR method applied to quartz grains, and especially of the potential and limitations of the Ti signals, it also provides additional baseline data to illustrate the existing variability among quartz samples of different origins or sedimentary context. Our results are consistent with previous studies by confirming that the Ti–H signal shows the best potential for the evaluation of low dose values (<100 Gy for these samples), whereas it becomes inappropriate for the higher dose range, and the Ti–Li–H (option D sensu Duval and Guilarte, 2015) should be used instead.Beyond the methodological outcome, this ESR dating study also provides a useful addition to the existing chronology of the aeolian deposits in this region. In particular, new (and possibly) finite numerical age results were obtained for the two oldest samples, constraining the aeolianite landward barrier dune and the coversand formations to the MIS 10-8 and Pliocene, respectively.     

Study on Buried Faults in the Weifang Urban Area

Buried faults in Weifang city and surrounding areas are studied with geophysical surveys such as shallow seismic survey and electrical exploration, and verified with engineering drilling. Six main faults are detected including the Yishul-Tangtou fault, Tangwu-Gegou fault, Hanting fault and Weixian fault, etc. The latest active age is determined by OSL, TL and ESR dating techniques. No active fault has been found so far in the Weifang urban area. Our results provide a scientific basis for land use and urban planning.     

Thermal stability and closure temperature of barite for electron spin resonance dating

Electron spin resonance (ESR) dating has been applied to barite from hydrothermal vents. Barite in hydrothermal vents cools down rapidly after formation so little attention was paid to the thermal stability of the ESR signal of barite for dating. To discern multiple episodes of fluid flow or to date barite in other geological settings, it is essential to know how the ESR intensity decays with heat, the characteristic decay time and the closure temperature. In this study, we demonstrate that the decay of the ESR intensity of the SO₃⁻ radical in barite is a second-order reaction. The characteristic decay time for the ESR intensity to drop by half at 100 °C, 200 °C, 300 °C and 500 °C is of the order of magnitude of 10⁶ years, 10 years, 10 h and 1 s respectively. The closure temperature of barite is generally between 190 and 340 °C. These results provide essential information on environments where the ESR intensity in barite is stable and conditions under which ESR ages can be erased.     

Insights into TT-OSL signal stability from single-grain analyses of known-age deposits at Atapuerca,Spain

Single-grain thermally transferred optically stimulated luminescence (TT-OSL) dating has recently been applied to a number of the Atapuerca palaeoanthropological sites. As yet, however, there have not been any direct assessments of TT-OSL signal stabilities for specific grains used for dating. In this study, we undertake a series of TT-OSL suitability assessments on known-age samples from Gran Dolina and Sima del Elefante. Our results suggest that the Atapuerca samples contain populations or sub-populations of grains with suitably stable TT-OSL signals for dating over late-Early and Middle Pleistocene timescales. Equivalent dose (D_e) distribution analysis in combination with pulse-annealing assessments provides a useful means of identifying inter-grain and inter-sample differences in TT-OSL signal stabilities. We also show that obtaining D_e values using different preheat conditions may help to identify potentially problematic TT-OSL behaviours. Analyses of multi-grain aliquot TL curves for these samples reveal that 'bulk' TL signal loss experiments may provide limited insights into TT-OSL source trap lifetimes due to averaging effects, the dominance of grain populations that do not produce TT-OSL, and interference from slowly bleaching OSL components. Our results improve the robustness and precision of existing TT-OSL chronologies for units TD6-3 and TE16-TE17 at Gran Dolina and Sima del Elefante, and support the broader suitability of the single-grain TT-OSL approach at the Atapuerca sites.     

热释光年代测定方法在鱼洞水库地区断层活动性研究中的应用

用作者研制的RS 81 1型热释光仪对云南昭通鱼洞水库地区两条断层的破碎带内发育的方解石脉进行了热释光年代测定和显微构造分析 .结果显示 :2条断层破碎带内发育 4期方解石脉 ,其中有 3期发生了变形 .F1 断层距今 5× 1 0 4 a以来 ,F2 断层距今 2 5× 1 0 4 a以来没有强烈活动的迹象 .断层泥中石英颗粒表面形态分析结果与热释光法相同 .