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.     

TL age-estimates for the Middle Palaeolithic layers at Theopetra cave (Greece)

The lowest stratigraphic unit of Theopetra cave (Greece) contains a Middle Palaeolithic sequence radiocarbon dated to between 46 and 35 ka BP; at the limit of this dating method. The upper part of this sequence has yielded late Middle Palaeolithic lithic assemblages containing several early Upper Palaeolithic artifacts. To get more precise dates for the human occupation of the cave, burnt flint specimens from these Middle Palaeolithic layers were dated by thermoluminescence. The dates obtained are coherent and indicate that the first human occupation of the cave took place at the end of isotopic stage 6 or more probably at the beginning of stage 5, much earlier than previously proposed. In the light of this new evidence, it is reasonable to assume that: (a) Theopetra contains the oldest dated Middle Palaeolithic deposits of Greece and (b) that the assemblages first interpreted as “Transitional Middle/Upper Palaeolithic” industries may be the result of post-depositional mixing of cultural material.     

Radiometric dates for the Middle Palaeolithic sequence of Payre (Ardèche, France)

The archaeological site of Payre (France) yielded Middle Palaeolithic layers with Neanderthal remains, which are partly bracketed by two stalagmitic flowstones. To obtain a precise chronological framework for the human occupation and the faunal remains of this site, several dating methods were used: uranium-series (U-series by alpha spectrometry and TIMS) and electron spin resonance (ESR) on stalagmitic flowstones, combined ESR/U-series on teeth and bones, and thermoluminescence (TL) on burnt flints. Most of the ages obtained for levels H to C range from 300 to 140 ka. The age-spread obtained for the anthropic (burnt flints) and faunal remains (bones and teeth) suggests that the dated levels represent several human occupation periods, near the transition from MIS8 to MIS7 (levels G–F) and from MIS6 to MIS5 (levels D–E).     

Extended-range luminescence chronologies for the Middle Pleistocene units at the Sima del Elefante archaeological site (Sierra de Atapuerca,Burgos, Spain)

The Sima del Elefante site is located within the Sierra de Atapuerca karst system (Burgos, northern Spain), and forms part of a series of important Early, Middle and Late Pleistocene archaeological complexes that have been dated previously with luminescence techniques (Gran Dolina, Galería Complex, Sima de los Huesos, Galería de las Estatuas). This study focuses on the upper Middle Pleistocene units (TE18 and TE19) at Sima del Elefante, which contain Acheulean and transitional lithic assemblages (Mode 2/3), as well as large and small mammal fossils. Importantly, these uppermost units are associated with a sediment plug located in the cave's interior at Galería Baja, which marks the closure of a significant palaeoentrance to the Atapuerca karst system. Establishing the accumulation history of these related deposits is important for understanding both Lower Palaeolithic technological dynamics via comparisons with similar levels at other Atapuerca sites (i.e., Gran Dolina and Galería Complex), as well as past human occupation patterns and carnivore use of (and accessibility to) the caves. We present single-grain TT-OSL and multi-grain pIR-IR chronologies for the Sima del Elefante upper sequence and the Galería Baja sediment cone, as well as U-series dating results for a stalagmitic crust capping the combined clastic infill sequence. The paired luminescence ages for the upper occupation levels are in agreement with each other and reveal that the host deposits accumulated 576–481 ka for the TE18 stratified scree layers, 266–237 ka for TE19 and 206–250 ka for the Galería Baja upper cone section (weighted mean 2σ age ranges). A concordant U-series age of 202 ± 65 ka is obtained for the overlying stalagmitic crust at Galería Baja. The Sima del Elefante ages are consistent with those previously obtained using U-series and biochronology, confirming that there is an erosional unconformity and complex carbonate deposition phase associated with the upper layers of unit TE18 and that the original cave entrance likely closed by ∼200 ka. Chronological correlation with other Atapuerca sites reveals potential equivalence between TE18 and unit TD8 (at Gran Dolina), and between TE19 and units GIIb–GIIIb (at Galería Complex) and, possibly, TD10.1 and TD10.2 (at Gran Dolina), though more refined dating is required to confirm the latter.     

Chronology of the Upper Pleistocene loess sequence of Havrincourt (France) and associated Palaeolithic occupations: A Bayesian approach from pedostratigraphy,OSL, radiocarbon,TL and ESR/U-series data

In connection with the future Seine-North Europe Canal (Seine-Scheldt), a large-scale rescue archaeological survey was conducted at Havrincourt (northern France) between 2008 and 2011. The discovery of several levels of Palaeolithic flint artefacts embedded in a relatively thick loess sequence (ca 6–7 m) preserved on a gentle slope facing North-East, resulted in a 6000 m² excavation. This opened the opportunity for a detailed pedosedimentary and interdisciplinary geochronological survey (¹⁴C, optically stimulated luminescence, thermoluminescence, ESR/U-series) that has allowed us date the sequence reliably. On the basis of these results we propose this sequence as a new pedostratigraphic and archaeological reference sequence for northern France. We present here the optical dating of the sequence performed on fine (4–11 μm) quartz grains extracted from 17 samples. The luminescence characteristics of these extracts indicate that the single-aliquot regenerative dose optically stimulated luminescence (SAR-OSL) procedure that was applied is well suited. A consistent set of optical ages was obtained for the loess deposited up to around 70 ka ago. Independent age control (pedostratigraphy, ¹⁴C, ESR/U-series dates) allowed us to apply a Bayesian approach to build a chronometric model. This in turn enabled a regional chronostratigraphic framework to be built, to constrain the correlations with neighboring regions (northern France and Belgium) and to calculate a precise age for the four Palaeolithic levels discovered, including a unique occupation related to the early Upper Palaeolithic which was previously unknown in the area.     

A targeted drilling and dating campaign to identify Stone Age archaeological sites before excavation in west coast southern Africa

Here we present the results of a targeted drilling campaign that facilitated a geochronological study with coarse sampling resolution inside a new cave site, Simons Cave, on the west coast of southern Africa. A combination of radiocarbon (¹⁴C) dating and optically stimulated luminescence (OSL) dating was used as a range-finder. Results confirmed preservation of Holocene and late Pleistocene sediments up to 133 ± 35 ka, overlapping with the ages of Middle Stone Age (MSA) occupations of the broader west coast region. A subsequent, systematic test-excavation at the site then embarked on a second geochronological study with a higher sampling resolution. Ultimately, the comparative study confirmed the potential of Simons Cave as a new site for the exploration of hominin occupation through the later Pleistocene and Holocene, yet raised several issues concerning the direct comparability of information deriving from drilled sediment cores and actual archaeological excavation.     

Optical dating of Holocene sand dune activities in the Horqin sand-fields in inner Mongolia, China, using the SAR protocol

The Horqin sand-field in northeastern Inner Mongolia, China, had been the fertile grassland in North China, but desertification and sand-dust storm have increasingly occurred in the past decades [Zhu and Wang, 1992. Theory and practice of sandy desertification in China (in Chinese with English abstract). Quaternary Sciences 2, 97]. To understand the Holocene sand dune activities in this region, five sand dune profiles were investigated, and 32 coarse grain quartz samples were dated by OSL using the single-aliquot regenerative-dose (SAR) protocol [Murray and Wintle, 2000. Luminescence dating of quartz using an improved single-aliquot regenerative-dose protocol. Radiation Measurements 32, 57–73]. For cross-checking, six organic-rich samples from the paleosols and sandy peat/mud were dated by both ¹⁴C and quartz OSL. With one exception, ¹⁴C and quartz OSL dating results show good agreements. Based on the consistent results of five sand dune profiles, a chronology of Holocene dune activity in Horqin sand-field is established as follows: (i) active sand dunes built up widely before 10 ka; (ii) dunes semi-stabilized between 10 and 7.5 ka ago; (iii) the dunes solidify and chernozem soils developed between 7.5 and 2.0 ka ago; and (iv) partially re-mobilization of dunes occurred since about 2.0 ka ago.     

Paleoflood events recorded by speleothems in caves

Speleothems are usually composed of thin layers of calcite (or aragonite). However, cemented detrital materials interlayered between laminae of speleothemic carbonate have been also observed in many caves. Flowstones comprising discontinuous carbonate layers form due to flowing water films, while flood events introduce fluviokarstic sediments in caves that, on occasion, are recorded as clayey layers inside flowstones and stalagmites. This record provides a potential means of understanding the frequency of palaeofloods using cave records. In this work, we investigate the origin of this type of detrital deposit in El Soplao Cave (Northern Spain). The age of the lowest aragonite layer of a flowstone reveals that the earliest flood period occurred before 500 ka, though most of the flowstone formed between 422 +69/‐43 ka and 400 +66/‐42 ka. This suggests that the cave was periodically affected by palaeoflood events that introduced detrital sediments from the surface as a result of occasional extreme rainfall events, especially at around 400 ka. The mineralogical data enable an evolutionary model for this flowstone to be generated based on the alternation of flood events with laminar flows and carbonate layers precipitation that can be extrapolated to other caves in which detrital sediments inside speleothems have been found. Copyright © 2014 John Wiley & Sons, Ltd.     

The chronology of the late Lower Paleolithic in the Levant based on U–Th ages of speleothems from Qesem Cave,Israel

We present here the results of a U–Th dating project at Qesem Cave, a Middle Pleistocene, late Lower Paleolithic site in Israel. It provides 54 new MC-ICP-MS U–Th ages for speleothems from the cave. The results indicate that human occupation started sometime between ～420 and 320 ka and ended between 220 and 194 ka. A survey of dates from culturally similar sites in the Levant indicates that the general range of ca. 400–ca. 200 ka is an appropriate estimate for the life span of the Acheulo-Yabrudian Cultural Complex (AYCC).     

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.     

Optical dating of St. Lawrence Iroquoian ceramics from the Mailhot-Curran site,southern Québec

Infrared-stimulated luminescence dating (IRSL) was applied on pottery sherds from the Mailhot-Curran archaeological site (BgFn-2), a Late Woodland period village located in the Saint-Anicet region, southern Québec (Canada). This site witnessed the presence of St. Lawrence Iroquoians and is thought to have been occupied roughly 500 years ago. The main goal of this study is to chronologically constrain the occupation of this site in order to establish a fine chronological sequence for the occupations of various sites found in this area. The IRSL is used to complement previous dating methods used for Mailhot-Curran (radiocarbon and seriation of the archaeological remains).Dating results are reported for ten samples of local ceramics made from Quaternary Champlain Sea clay. Luminescence dating on fine grains was preferentially used, since feldspar luminescence typically emit a decent luminescence signal. Although the latter was rather dim, anomalous fading was measured and luminescence ages were successfully corrected. It is therefore possible to validate the occupation age of this site.     

230Th/U chronology of a paleolithic site at Xinglong Cave in the three-Gorge region of south China

Xinglong Cave, containing four human teeth, numerous mammalian fossils, stone artifacts and a Stegodon tusk with intentional and seemingly grouped engravings, is one of the most significant archaic Homo sapiens sites in south China, located 95 km south of Fengjie County, in Chongqing. In an attempt to constrain the age of the human relics, calcitic flowstone deposits with a significant detrital component were dated by U–Th methods using a leachate scheme. Total sample digestion MC-ICPMS dating was used to assess the reliability of the leachate technique. Six calcite samples from horizons beneath and above the fossil-bearing layer were dated. We obtained ages of 130 ± 9.1, 124 ± 11, 135 ± 12 and 127 ± 11 ka for the flowstones above the fossil layer with a weighted mean of 128.9 ± 5.2 ka. Two flowstone samples gave MC-ICPMS dates between 128.3 ± 3.3 and 152.4 ± 25.3 ka with an assumed detrital component to correct for the initial ²³⁰Th, which are consistent with results obtained using the L/L regression data from layer U-4 within uncertainty. All errors herein quoted at the 2σ level. Ages determined for the flowstone underlying the fossil-bearing layer were 221 ± 29 to 189 ± 19 ka with a weighted mean age of 199 ± 16 ka. These results are stratigraphically consistent within error limits and show that the cave was occupied by Fengjie Man within the time range of ∼200 to ∼130 ka. These new U-series ages of flowstones in association with human teeth and an engraved stegodon tusk at the Xinglong Cave site provide valuable geochronologic information for the study of the origin of modern humans in East Asia and earliest human art.     

New ESR/U-series dates of the lowest Acheuleo-Yabrudian levels of Qesem cave

Qesem cave is a Middle Pleistocene site located close to Tel Aviv, Israel, assigned to the Acheuleo-Yabrudian Cultural Complex (AYCC) of the Lower Palaeolithic. The site provides rich assemblages of knapped flint, animal remains and some human teeth making it of particular interest. Its location in the Levantine corridor confers a major interest to the understanding of human dynamics during the Middle Pleistocene.A series of 6 herbivorous teeth from the base of the 11 m archaeological sequence of AYCC Qesem Cave was analysed by combined ESR/U-series method; this complements previous dating series carried out on teeth and on heated flints on higher parts of the sequence (Mercier et al., 2013; Falguères et al., 2016) The teeth were measured according a regular protocol for which each tissue was analysed by inductively coupled plasma-quadrupole mass spectrometry (ICP-Q-MS) for U-series using a combination of a Thermo iCAP-RQ mass spectrometer coupled to a Cetac Aridus III desolvator system, and ESR analyses were implemented on enamel tissue. All these data were combined in order to yield modelled ages.The goal was to find out whether there was a time gap between the carbonates layers dated to 420 ka (Gopher et al., 2010) and archaeological layers of the AYCC found throughout the cave's sequence. The new results yield ages ranging between 220 and 430 ka confirming a great antiquity and a long duration of AYCC in the Levant.     

Luminescence dating of ephemeral stream deposits around the Palaeolithic site of Ifri n'Ammar (Morocco)

The prehistoric site of Ifri n'Ammar is situated in northeastern Morocco, in the northern prolongation of the Middle Atlas Mountains. It is a key location in unravelling the history of anatomically modern humans (AMH) in northern Africa as it reveals Middle and Late Palaeolithic occupation phases since ∼170 ka. Whilst the archaeological sequence within the rock shelter has been well studied, the timing of landscape dynamics around Ifri n'Ammar is still poorly understood. This study therefore aims to establish a detailed chronology of the Wadi Selloum profile at the apron of the shelter, based on optically stimulated luminescence (OSL) dating of ephemeral stream deposits. Coarse-grain quartz was used for single-grain and multiple-grain dating procedures to investigate the luminescence properties of these deposits and to get more accurate age information concerning the phases of human occupation. Continuous wave OSL (CW-OSL) revealed a dominant fast component for all quartz samples. The dose distribution of the uppermost samples showed overdispersion values >25% and significant positive skewness. We identified partial bleaching as the main source of scatter in the equivalent dose (D_e) distribution. The lowermost sample appeared to be close to signal saturation. The shapes of the dose response curve varied widely between aliquots and coarse quartz grains exhibited therefore very different dose saturation behaviours among aliquots. With fully saturated dose response curves (DRCs), meaningful D₀ values were assumed for D_e estimation.The eight OSL samples yielded stratigraphically consistent ages ranging from 1.3 ± 0.2 ka to 76 ± 5 ka, thus reaching the Middle Palaeolithic period. Moreover, a pottery shard dated to 7.4 ± 0.6 ka (Early Neolithic period) by thermoluminescence (TL), perfectly matched the Holocene OSL samples extracted at the same depth of the profile. In summary, our results point to fluvial aggradation during OIS 5.1, the late glacial period, and the Holocene.     

Testing a new combined (U,Th)–He and U/Th dating approach on Plio-Pleistocene calcite speleothems

The geochronology of cave deposits in the Cradle of Humankind UNESCO World Heritage Site in South Africa provides a timeframe essential for the interpretation of its fossils. The uranium-lead (U–Pb) and uranium-thorium disequilibrium (U/Th) dating of speleothems, mostly flowstones that underlie and blanket the fossil-bearing sediments, have been effective in this sense, but U–Pb is limited by the requirement of ∼1 ppm U concentrations and low common Pb contents, and U/Th has a c. 500 ka limit of applicability. Here we report age results for calcite-aragonite speleothems obtained using a new combined uranium-thorium-helium ((U,Th)–He) and U/Th dating routine. We reproduced within analytical uncertainty, the published U–Pb or U/Th ages for (a) flowstone in three drill core samples in the range 2000–3000 ka, (b) a flowstone hand sample taken at surface with an age of 1800 ka, and (c) five underground flowstone samples in the range 100–800 ka. Calcite retentivity for He under cave conditions is thus demonstrated. In the few cases where helium loss was observed in speleothems, only some of the subsamples were affected, and to varying degrees, suggesting loss by lattice damage not related to diagenetic processes, rather than volume diffusion. In the 100 to 800 ka range, the combined U/Th disequilibrium and (U,Th)–He method also yielded reliable values for initial (²³⁰Th/²³⁸U) and (²³⁴U/²³⁸U) activity ratios. Importantly, most subsamples had high initial (²³⁰Th/²³⁸U) values, ranging from 1.0 to 19.7, although having low Th/U ratios. This is probably due to incorporation of Fe–Mn oxides-hydroxides dust, on which ²³⁰Th was previously adsorbed. Such samples are mostly not dateable by U/Th without the additional input from the He analysis. If not detected and corrected for, such high initial (²³⁰Th/²³⁸U) values can lead to inaccurate U/Th and U–Pb ages. Our study shows that the incorporation of He analysis in U/Th dating has broad potential application, with four methods for calculating the ages, in carbonates from different environments where U-Pb or U/Th dating would not work.     

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.     

ESR dating of dental enamel from Middle Palaeolithic levels at Lazaret Cave,France

ESR dating was carried out on Cervus elaphus tooth enamel samples from the depositional sequence of Lazaret Cave, Nice, France. The deposits contain Anteneandertal hominid fossils associated with abundant lithic artefacts and faunal remains. Three samples from the Mousterian occupations in complex CIII (Fouille d'entrée) yielded early uptake (EU) ages between 108 and 125 ka and linear uptake (LU) ages between 133 and 160 ka. Seven samples from the Acheulian levels in the upper part of the complex CII (Fouille d'entrée and Fouille centre) gave EU ages between 113 and 165 ka and LU ages between 147 and 210 ka, with weighted means at 131 ± 7 and 165 ± 9 ka, respectively. The results of six enamel samples from the lower Acheulian levels at Locus VIII, another place in the cave, were discarded because of their decreasing tendency with depth. The US–ESR combination method was also applied and the CSUS–ESR dates were calculated using the ESR-DATA program. Altogether, the data suggest that the Lazaret Acheulian and Mousterian occupations were rapidly formed during OIS 6.     

Luminescence dating of old (>70 ka) Chinese loess: A comparison of single-aliquot OSL and IRSL techniques

The applicability of two different approaches in the luminescence dating of old (>70 ka) Chinese loess is investigated. Both SAR-OSL ages obtained on 63–90 μm quartz grains and SAR-IRSL ages obtained on 4–11 μm polymineral grains, for samples collected from two sites in the Chinese Loess Plateau (Luochuan and Dongchuan) are presented. The characteristics of the luminescence signals stimulated by blue and infrared light are investigated in terms of dose response and dose recovery, and as a function of age. Additionally, anomalous fading measurements from the 410 nm IRSL emission in polymineral fine-grains are reported. An average value of g_2days amounting to 3% per decade was measured and seems to be independent of site location and age. For the samples from Luochuan, independent age control (pedostratigraphy and palaeomagnetism) is available. At both sites, the SAR-OSL ages are always lower than the SAR-IRSL ages after they have been corrected for anomalous fading. It seems that the quartz-based SAR-OSL ages are accurate for the younger ages, but that they underestimate the true age of deposition for loess that was deposited about 60–70 ka ago. The fading-corrected SAR-IRSL ages are in better agreement with the pedostratigraphic age control (75 and 130 ka) and allow dating beyond the quartz OSL range. Based on our results, we suggest that conventional SAR-OSL and SAR-IRSL protocols at these sites should be restricted to samples of ages not exceeding 40–50  and 100–120 ka, respectively.     

New ESR and U-series dating at Caune de l'Arago,France: A key-site for European Middle Pleistocene

The Caune de l'Arago, located at Tautavel in the southern part of France, is one of the best documented Middle Pleistocene sites allowing a good understanding of human evolution in Europe. Since its discovery in 1829, the cave yielded more than 140 human remains associated with abundant lithic industries and thousands of faunal remains in a 10 m thick stratigraphical sequence divided in three complexes (Lumley et al., 2014). The Lower stratigraphic complex is only known from cores while the Middle and Upper ones can be divided into about 17 main archaeological levels indexed from the bottom to the top: from level Q to level A. Since 1981, a number of dates were done using practically all the methods available for dating Quaternary period up to 700 ka. U-series dates performed on the upper stalagmitic floor yielded a minimum age of 400 ka for human remains found in the underneath level G (Falguères et al., 2004). This age range confirmed the direct non-destructive gamma-ray age published more than 30 years before (Yokoyama and Nguyen, 1981). Recently, a methodological work was published on herbivorous teeth coming from different parts of the G level highlighting the difficulties to get reliable radiometric dates on a level so rich in bones and partly weathered by guano deposits or issues associated with carbonate accumulation (Han et al., 2010).This study presents new ESR/U-Series dates obtained on herbivorous teeth coming from the lowest excavated layers (Q–P levels) which yield an age range for the entire thick archaeological infilling. The new results suggest that the sedimentological levels containing lithic and faunal artefacts began to be deposited at 550 ka in the P–Q levels and a younger age of 350–400 ka for the F level. The P–Q levels which have yielded bifaces are one of the oldest evidence of the Acheulian culture in the southern part of Western Europe while the dates obtained on G level suggest a contemporaneity with la Sima de los Huesos and TD10 Dolina level at Atapuerca.