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.     

Evaluation of ESR residual dose in quartz modern samples,an investigation on environmental dependence

Luminescence and ESR dating methods of quartz sediment are based on the natural resetting of the signal by light exposure (optical bleaching). When the bleaching is incomplete, a residual dose (D_eR) is added to the post-depositional dose accumulated since the deposit and hence the age is overestimated.Insufficient bleaching is usually linked to the environment and conditions of transport/deposition of the quartz grains affecting the light exposure duration. Indeed, each transportation mode – fluvial, marine or aeolian – is associated to specific conditions of light exposure, depending mainly to the location of grains in the transport agent during the transport phase, the opacity of the transport environment and the velocity of the transport.The present study attempts to discriminate the modes of transport/deposition providing a satisfying reset of the ESR signals of quartz grains. For this purpose, we investigated bleaching rates and ESR residual doses of aluminum centers from “present-day” aeolian, fluvial and marine sediments sampled in various sedimentary environments. The bleaching efficiency evaluation in these different environments may help for a better understanding of the resetting phenomenon for quartz signals which represents presently the main difficulty for ESR dating.The results show that the residual doses are small enough to allow an ESR dating of the main part of the sediment transported in almost all the context examined in this study. The smallest residual doses are obtained from quartz grains within the range of 100–200 μm and transported in clear water. Some limits for the application of optically bleached quartz ESR dating appears nevertheless, mainly when the residual dose and the dose accumulated after the deposit are quite similar, i.e. for Upper Pleistocene samples.     

Effects of grain size on quartz ESR dating of Ti–Li center in fluvial and lacustrine sediments

The electron spin resonance (ESR) dating method has been introduced into the Quaternary chronology for nearly 40 years and has been successfully used for dating of fluvial and lacustrine sediments. In order to evaluate the possible effect of the sediment grain size on the dating estimate, the parallel ESR dating testing was carried out on quartz grains of five different size fractions ranging from 50 to 450 μm extracted from the same fluvial and lacustrine sediment collected close to the M/B boundary at the Donggutuo section, Nihewan Basin, China. The results show that equivalent doses and associated ages vary significantly. However the beta irradiation dose rate of the grains with different sizes accounts for only about 6% of the total deviation of the dating results. At the same time, the sensitivity of quartz Ti–Li center was calculated based on the additional irradiation. It shows that the larger grains are more sensitive than the smaller ones, which can leads to higher saturate ESR intensity and less equivalent dose. The variations of the sensitivity of quartz Ti–Li center of the grains with different sizes are responsible for the primary deviation of the dating results. The results also suggest that 100–150 μm grain size fraction would be priority size for the ESR dating of quartz Ti–Li center on fluvial and lacustrine sediments.     

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 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.     

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     

第四纪沉积物ESR年代学研究进展

在缺少第四纪火山活动的区域,沉积物成为第四纪地质构造和地貌、环境演化等方面研究的主要年代学测量对象.对于老于200ka的沉积物,电子自旋共振(ESR)是潜在的测量方法之一.ESR信号中心会在光晒退或热事件的作用下衰减或"回零".对于第四纪沉积物而言,在最后一次埋藏事件发生之前,只存在阳光晒退作用,因此了解各ESR信号中...     

ESR dating of fluvial quartz: Estimate of the minimal distance transport required for getting a maximum optical bleaching

An ESR experimental study of artificial optical bleaching of sedimentary quartz has shown that the aluminum center was maximally bleached after a 6-month illumination equivalent to natural light. This duration seems too long to apply in natural conditions. Nevertheless, the measurement of the ESR intensity of aluminum centers in quartz extracted from modern sediments and deposited in sandy bars shows that the maximum bleaching has effectively been reached.

In order to determine the relationship between the bleaching and the distance covered by a quartz grain in a river, samples were collected along the Creuse River (France) from its spring to about 170 km downstream, where maximum bleaching levels were observed in previous studies. The ESR intensities of the aluminum and titanium centers in quartz were measured, using X-band spectroscopy, before and after artificial bleaching. The difference measured between these sub-samples shows that the maximum bleaching level is obtained in the course of the first kilometer. Hence, the assumption that ESR dating of fluvial sediment is based on the optical bleaching was validated.     

On the interest of using the multiple center approach in ESR dating of optically bleached quartz grains: Some examples from the Early Pleistocene terraces of the Alcanadre River (Ebro basin,Spain)

The present work reports the first numerical ages obtained for the two highest fluvial terraces (Qt1 and Qt2) of the Alcanadre River system (Northeastern Spain) representing the earliest remnants of Quaternary morphosedimentary fluvial activity in the Ebro basin. ESR dating method was applied to optically bleached quartz grains and both the Al and Ti centers were measured, in accordance with the Multiple Center approach. The results are overall in good agreement with the existing preliminary chronostratigraphic framework and our interpretation indicate that terraces Qt1 and Qt2 have an ESR age of 1276 ± 104 ka and 817 ± 68 ka, respectively. These data provide some chronological insights on the beginning of the fluvial sedimentary processes in a scenario of incision maintained over Quaternary in the Ebro Basin. These are among the first numerical ages obtained for such high terraces in the Iberian Peninsula.Our results demonstrate the interest of using the Multiple Center approach in ESR dating of quartz, since the two centers provide complementary information, i.e. an independent dose control. The overall apparent consistency between the ESR age estimates and the existing preliminary chronostratigraphic framework may be considered as an empirical evidence that the Ti–Li center may actually work for Early Pleistocene deposits, whereas the Ti–H center shows some clear limitations instead. Finally, these results demonstrate the interest of using ESR method to date Early Pleistocene fluvial terraces that are usually beyond the time range covered by the OSL dating method.     

ESR dating of quartz phenocrysts in the El Cajete and Battleship Rock Members of Valles Rhyolite, Valles Caldera, New Mexico

The electron spin resonance (ESR) dating method was employed on quartz phenocrysts separated from pumice of the El Cajete and Battleship Rock Members of the Valles Rhyolite in the Valles caldera, New Mexico. The results of heating experiments indicate that Ti impurity centers have two components; a thermally stable one and a less stable, temperature sensitive one. ESR dates using the stable Ti center yield eruption ages of 59 ± 6 ka for the Battleship Rock Member and 53 ± 6 ka for the El Cajete Member while recent ¹⁴C dates (S. Reneau and J. Gardner, unpub. data) from carbonized logs in the El Cajete pumice indicate that its age is older than 50 ka. Our results indicate that volcanism in the Valles caldera is much younger than previously thought (≥ 130 ka) and that recent revisions to the post-0.5 Ma stratigraphy of Valles caldera are probably in error. The results suggest that ESR dating of quartz may be a useful method for obtaining ages of units in other Quaternary volcanic areas.     

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.     

沂沭断裂带大水场剖面断层泥的ESR年代学研究

对山东省沂水县大水场断层剖面的断层泥带进行了野外观测和ESR 测年。断层泥的ESR年龄与由其穿插关系等判断出的断层活动次序相符。各断层泥的ESR 年龄显示出大水场断层经历了两个活动较频繁的时段,即0-25～0-28Ma B-P- 和0-45～0-55Ma B.P     

ESR chronology of the Somme River Terrace system and first human settlements in Northern France

The Somme Valley, Northern France, is famous for its archaeological sequence, where numerous rich Palaeolithic sites, such as Saint-Acheul, the type site of the Acheulian, have been discovered. The archaeological levels are often directly associated with fossil alluvial sediments of the River Somme or with slope deposits, including loess and palaeosols. In the middle reaches of the valley, near Amiens, the system of fossil-stepped fluvial terraces is particularly well developed and preserved, and occurs on 10 alluvial formations. These terraces, from +5 to +55 m above the present-day valley bedrock, allow the study of the environmental changes and the human settlement of this area through the Pleistocene.

Since 1988, ESR dating was systematically applied on bleached quartz extracted from the fossil fluvial deposits, in order to better describe the geological evolution of the stepped system. More recently, U-series/ESR dating has also been performed on teeth collected from the different terrace deposits. Here we present a synthetic review of the main ESR results, and propose an ESR chronology for the geological evolution of the Somme fluvial system and for the Middle Pleistocene human settlement of northern France.     

Radiometric dating of Meipu hominin site in China by coupled ESR/U-series and cosmogenic 26Al/10Be burial dating methods

The Three Gorges and Western Hubei area in the geographic central part of China was a potential migration corridor for early hominin and mammals linking South and North China during the Pleistocene period. Some key early hominin sites are known in this region where limestone cave and fissure sites are numerous but difficult to date as beyond the dating range of OSL and mass spectrometry U-series method. Here, we report radiometric dating study for such a hominin site, Meipu (Hubei Province), by coupled ESR and U-series dating of nine fossil teeth and cosmogenic ²⁶Al/¹⁰Be burial dating of one quartz sediment. The burial age calculated by simple burial model (573 ± 266 ka) gives a minimum age constraint of the sediment. The fossil dating provided two main age groups at 541 ± 48 ka and 849 ± 39 ka, the older age group is in agreement with the U-series age (>630 ka) of the flowstone overlying the fossil layer and the paleomagnetic data which placed the Brunhes-Matuyama boundary in the fossil layer. The reason of this age difference is probably caused by the U-content discrepancy in the enamel of the dated fossil samples. This study exhibits the limitation of ESR/U-series fossil dating and the importance of using multiple dating approach when it is possible in order to identify the problematic ages.     

Electron spin resonance dating of optically bleached quartz grains from the Middle Palaeolithic site of Cuesta de la Bajada (Spain) using the multiple centres approach

Electron spin resonance (ESR) dating of optically bleached quartz grains was performed on three sediment samples collected from the Middle Palaeolithic site of Cuesta de la Bajada (Spain). A standard multiple grain and multiple aliquot additive dose procedure was employed, and both the Al and Ti centres were measured as part of the multiple centres approach.ESR age estimates obtained for the three samples indicate that the Al centre provides a maximum possible chronology, as the Ti centres show that the Al signal was likely not systematically reset to its residual level during sediment transport. A direct comparison between ESR ages based on the Ti centres and single grain optically stimulated luminescence (OSL) ages from samples collected nearby shows broadly consistent results. The Ti-H centre also appears to provide suitable chronologies for at least two of the three Middle Pleistocene samples studied here. Surprisingly, the only sample showing consistent ESR ages between the Al and Ti centres appears to be overestimated in comparison with the Ti-centre and OSL ages derived from the other two samples. This indicates either incomplete bleaching of both the Al and Ti centres for this sample, or unexpected impacts of other sources of D_e uncertainty, such as multi-grain averaging effects. The ESR dating results overall indicate that the archaeological sequence of Cuesta de la Bajada CB-3 is most likely correlated to either MIS 7 or 9.     

ESR chronology of alluvial deposits in the Arlanzón valley (Atapuerca,Spain): Contemporaneity with Atapuerca Gran Dolina site

The Sierra de Atapuerca (Northern Spain) is characterized by a well-developed karst system where several major archaeological sites have been discovered, attesting an almost continuous hominin occupation of the area during the whole Pleistocene period. Previous geomorphological studies showed a connection between genesis of the karst system and the evolution of the nearby Arlanzón river Valley. However, numerical dating results were missing to refine the chronostratigraphical framework of the Arlanzón valley's fluvial incision. To address this, we applied the Electron Spin Resonance (ESR) dating method to sedimentary optically bleached quartz grains from several fluvial terraces. Nine samples were collected from five of the 14 identified terraces. The ESR age results are stratigraphically coherent and in general agreement with both previous geomorphological observations and available palaeomagnetic data. Consequently, an ESR chronology of the geological evolution of the Arlanzón valley is proposed, which can be then correlated to the sedimentary sequence of the palaeoanthropological site of Atapuerca Gran Dolina. Our results provide important information about the chronology of hominid occupation in this area during Early and Middle Pleistocene.     

ESR dating of sedimentary quartz: Possibilities and limitations of the single-grain approach

Usually, multiple-grain aliquots are used for electron spin resonance (ESR) dating of sediments. However, this approach excludes the ability of detecting insufficient bleaching, as would be the case when measuring several single aliquots or single grains. In this paper, we present preliminary results of single-grain ESR dating experiments on three different sedimentary deposits (fluvial, fluvio-aeolian and desert aeolian), ranging in age between 100 ka and 2 Ma. Titanium-related impurity centres (Ti–Li and Ti–H) were measured in a Q-band ESR spectrometer for estimating equivalent doses (D_e) of individual quartz grains (0.5–1 mm). Both additive and regenerative dose methods were used. The resulting D_e plots show a large scatter in D_e—from 100 Gy to more than 600 Gy—for the fluvial sample, probably reflecting different bleaching histories of the grains. On the contrary, a clear plateau can be observed in D_e for sands with a strong aeolian component. Preliminary single-grain ESR ages are in relatively good agreement with independent estimates, the best results being obtained for the desert aeolian sample (200 ka). It is concluded that ESR has a promising potential for estimating large naturally accumulated doses of well-bleached sediments. Nevertheless, the method is challenged by several experimental difficulties, such as long measurement times, excessive errors, and presumably a complex interrelationship between Ti–Li and Ti–H components.     

黄河小浪底水库区断层的ESR年龄测定

为了检验应用ESR方法测定断层运动年龄的可行性,在黄河小浪底水库区内的5个断层剖面上采集了13个样品进行ESR年龄测定。结果指出;研究区内的断层活动大致发生于距今0.154—0.183Ma及0.374—0.532Ma两个时期。并对一些有关问题作了讨论,指出这是一种很有希望的确定断层活动近似年龄的新方法,在地震地质及工程地质领域中具有良好的应用前景     

Dating of Japanese Quaternary tephras by ESR and luminescence methods

Electron spin resonance (ESR) and red thermoluminescence (RTL) methods were applied to quartz of eight Japanese Quaternary tephras ranging from 30 to 900 kyr, which have independent ages from other dating methods. The ESR ages were consistent for younger samples, while those from the Ti–Li center are older than those for the Al center for older samples. RTL ages are consistent with the age references and are roughly consistent with Al center ages. The dose response of the Ti–Li center after heating at 260 °C for 15 min implies that thermally unstable component is created in Ti–Li center by irradiation, leading to possible overestimations in the dose values.     

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.