ESR dose response of Al center measured in quartz samples from the Yellow River (China): Implications for the dating of Upper Pleistocene sediment

The ESR dating method requires to describe the evolution of the ESR signal intensities vs. increasing gamma doses, then to extrapolate the equivalent dose of radiation received by the sample since its deposition using mathematical fitting. The function classically used to describe the growth curves of ESR aluminium signal in quartz was recently discussed and challenged for Lower Pleistocene sediments. In the present work, some alluvial sediments sampled in Upper Pleistocene fluvial terraces of the Yellow River system (China) permit us to test the application of another extrapolation function (linear + exponential) recently proposed for Lower Pleistocene sediments. The equivalent doses obtained here for the recent deposits of the Yellow River system and the corresponding ages are promising and indicate the potential of ESR to date quartz deposits from Upper Pleistocene times.     

ESR Dating of Tooth Enamel: Comparison with AMSC at El Castillo Cave, Spain

At El Castillo, in Cantabrian Spain, uncalibrated AMS¹⁴C dating has shown the transition from Mousterian to Aurignacian to occur at 39·3±1·6 kaBP. We found ESR tooth enamel ages from the basal Aurignacian level at El Castillo to be 36·2±4·1 ka (early and linear uptake). The enamel and dentine had very low U contents, but ESR ages are strongly dependent upon knowledge of the moisture content history of the sediments. Although the Aurignacian ESR age is 8% younger than the weighted average uncalibrated AMS¹⁴C age of 39·6±1·3 ka obtained from charcoal samples, we have shown that the methods agree within experimental uncertainty. However, since no precise¹⁴C calibration yet exists for this period of time, we are unable to specify which of the ages is more accurate, nor are we able ascribe the apparent age discrepancy to a particular deficiency in the ESR method.     

New radiocarbon dating of the transition from the Middle to the Upper Paleolithic in Kebara Cave,Israel

The Middle to Upper Paleolithic transition (MP-UP transition) is considered a major technological and cultural threshold, at the time when modern humans spread “out of Africa”, expanded from the Levant into Europe and possibly into central and northern Asia. The dating of this techno-cultural transition has proved to be extremely difficult because it occurred sometime before 40,000 radiocarbon years before present (¹⁴C years BP), which is close to the end of the effective dating range of radiocarbon. Other dating methods such as Thermoluminescence (TL) or Electron Spin Resonance (ESR) are not sufficiently precise to date the recorded archaeological MP-UP transition in the Levant. Here we report a consistent set of stratified radiocarbon ages on freshly excavated charcoal from Kebara Cave, Mt. Carmel (Israel), that span the late Middle Paleolithic (MP) and Early Upper Paleolithic (EUP) This study applied novel strategies to improve sample preparation techniques and data analysis to obtain high-resolution radiocarbon models. From this study it is proposed that the MP-UP transition for this site can be placed immediately after 45,200 ± 700 ¹⁴C years BP and before 43,600 ± 600 ¹⁴C years BP or from 49/48 to 47/46 radiocarbon calibrated years before present (years Cal BP).     

ELECTRON SPIN RESONANCE ANALYSIS OF MARINE GASTROPODS FROM COASTAL ARCHAEOLOGICAL SITES IN SOUTHERN AFRICA

Shell samples of the marine gastropod Turbo sarmaticus have been examined to assess their potential for electron spin resonance (ESR) dating. The shells were found to be composed of aragonite. ESR analysis shows the presence of three radiation sensitive peaks. Equivalent dose (ED) values for two of the peaks have been determined for thirteen samples. When the two sets of ED values are plotted against each other, four distinct clusters are found that appear to represent four different age groups. The apparent age groups determined here are consistent with the stratigraphic record of the sites.     

IRSL and post-IR IRSL residual doses recorded in modern dust samples from the Chinese Loess Plateau

Using a set of modern/young (0 to about 200 years old) dust samples collected from the Chinese Loess Plateau the bleachability of IRSL measured at 50°C (IR₅₀) and post-IR₅₀ elevated temperature IRSL (measured at 225°C and at 290°C) is investigated by measuring the apparent (residual) doses recorded by these signals. Doses recorded by quartz OSL are used as a reference. Allowing for differences in dose rates it seems that both IRSL and post-IR IRSL signals yield residual doses that are significantly larger than the doses measured in quartz. These residual doses can be largely explained by thermal transfer caused by preheating. Nevertheless, we advise against the use of a low temperature preheat (<200°C) with IR₅₀ to date loess samples because, as has been reported before, the signal appears to be thermally unstable. In general, we conclude that it may not be advisable to apply post-IR IRSL dating to Chinese loess samples where residuals of up to ∼20 Gy are a significant fraction of the total dose. However, these residuals quickly become unimportant when dating older samples, and this is the age range in which post-IR IRSL dating is likely to be most useful.     

ESR dating of the Donggutuo Palaeolithic site in the Nihewan Basin, northern China

The fluvio-lacustrine sequences in the Nihewan Basin, northern China, provide important terrestrial archives about Palaeolithic settlements and, therefore, about early human occupation in high northern latitude in East Asia. Here we present detailed ESR dating of the Donggutuo Palaeolithic site, located in this basin. Four levels A, B, C and E of the Donggutuo archaeological layer yield ESR ages ranging from 1060±129 ka to 1171±132 ka with a mean of 1119±132 ka. The ages are consistent with the paleomagnetic data, which show that the Donggutuo Palaeolithic site lies just below the onset of the Jaramillo normal subchron (0.99–1.07 Ma). Furthermore, our results indicate that the reliable ESR dating range of bleached quartz using Ti-Li centre can be effectively extended to 1100 ka and the Ti-Li centre was zeroed before the last deposition, which requires improvement of the understanding of the bleaching mechanism conditions.     

Mass spectrometric U-series dating of Laibin hominid site in Guangxi, southern China

The Laibin hominid represents one of the rare finds of modern Homo sapiens in China, rare for its relative completeness and well-established stratigaphic provenance. This paper presents the results of mass spectrometric U-series dating of intercalated calcite samples from the Laibin site. The capping flowstone and the calcite vein, which sandwich the hominid fossil-containing deposits, date to 38.5 ± 1.0 and 44.0 ± 0.8 ka, setting respectively the minimum and maximum ages to the fossils. The second flowstone layer is 112.0 ± 1.4 ka old, indicating that the cultural sequence may possibly extend to somewhere between 44 and 112 ka. Securely dated Laibin finds should be of importance in reconstructing human physical and cultural evolution in the region.     

The E<Subscript>1</Subscript>’ center in natural quartz: Its formation and applications to dating and provenance researches

Quartz is one of the minerals useful for electron spin resonance (ESR) dating. The E₁′ center is one of well-known paramagnetic defects in crystalline quartz. This center has a unique feature; its intensity increases on heating. An electronic process to explain this increase was found to be controlled not only by the number of oxygen vacancies, which are the precursors, but also by the number of Al hole centers, which depend on the previous radiation dose and on the Al concentration.     

Detailed protocol for an accurate non-destructive direct dating of tooth enamel fragment using Electron Spin Resonance

In the context of human evolution, fossil remains are too valuable to be destroyed and any alteration should be kept to a minimum. The newly developed protocol on fossil fragments has open the gate for ‘virtually’ non-destructive ESR (Electron Spin Resonance) direct dating of human remains. The method allows the separation of unstable and interfering signals that were responsible for large dose underestimation. While a complete investigation of the ESR signal remains a complex task and requires numerous hours of manipulations, a rapid dose assessment protocol can be achieve without compromising the accuracy nor the integrity of the sample. The new protocol should be used for future dating regardless of the possibility of measuring powder.     

U-series Dating of Fossil Teeth and Carbonates from Snake Cave,Thailand

Snake Cave (Thailand) is an important site for the study of the evolution in Southeast Asia, leading to a discovery of rich and various faunas, including a human tooth. Fossils of large and small mammals converge to indicate, on the basis of faunal assemblage, a late Middle Pleistocene age for the fossiliferous layers; on the other hand, previous U-series dating of carbonates furnished a lower limit for the fossils of about 130 ky.In order to achieve a better comprehension of the chronology of the cave, the Uranium-series method for absolute age determination has been applied to some carbonates older than those studied previously and to fossils themselves.We used the isochron technique approach to yield valuable ages because spleleothem samples consist in a mixture of calcite and detrital contamination. The results obtained suggest that the main fossiliferous level is older than about 160 ky. The application of the U-series method to tooth samples from this tropical cave leads to erroneous ages, probably because of post depositional groundwater movements.     

DATING OF THE HOMINID (HOMO NEANDERTHALENSIS) REMAINS ACCUMULATION FROM EL SIDRÓN CAVE (PILOÑA,ASTURIAS, NORTH SPAIN): AN EXAMPLE OF A MULTI‐METHODOLOGICAL APPROACH TO THE DATING OF UPPER PLEISTOCENE SITES

The age of Neanderthal remains and associated sediments from El Sidrón cave has been obtained through different dating methods (¹⁴CAMS, U/TH, OSL, ESR and AAR) and samples (charcoal debris, bone, tooth dentine, stalagmitic flowstone, carbonate‐rich sediments, sedimentary quartz grains, tooth enamel and land snail shells). Detrital Th contamination rendered Th/U dating analyses of flowstone unreliable. Recent ¹⁴C contamination produced spurious age‐values from charcoal samples as well as from inadequately pretreated tooth samples. Most consistent ¹⁴C dates are grouped into two series: one between 35 and 40 ka and the other between 48 and 49 ka. Most ESR and AAR samples yielded concordant ages, ranging between 39 and 45 ka; OSL dating results permitted adequate bracketing of the sedimentary layer that contained the human remains. Our results emphasize the value of multi‐dating approaches for the establishment of reliable chronologies of human remains.     

ESR dating of the Neanderthal site, Kebara Cave, Israel

In 1985 a Neanderthal skeleton was found in the cave of Kebara in southern Mt. Carmel. Electron spin resonance (ESR) dates have been obtained on tooth enamel of gazelles found in layer X, just overlying the layer in which the skeleton was found. Assuming early uptake of uranium by the teeth, they yield an age of 60 ± 6 ka; assuming gradual, linear uptake of uranium yields an age of 64 ± 6 ka. Both age estimates are consistent with a previous estimate for the skeleton, based on TL dating of burnt flint, of 60 ± 4 ka.     

Investigating the resetting of OSL signals in rock surfaces

There are many examples of buried rock surfaces whose age is of interest to geologists and archaeologists. Luminescence dating is a potential method which can be applied to dating such surfaces; as part of a research project which aims to develop such an approach, the degree of resetting of OSL signals in grains and slices from five different cobbles/boulders collected from a modern beach is investigated. All the rock surfaces are presumed to have been exposed to daylight for a prolonged period of time (weeks to years). Feldspar was identified as the preferred dosimeter because quartz extracts were insensitive. Dose recovery tests using solar simulator and IR diodes on both K-feldspar grains and solid slices taken from the inner parts of the rocks are discussed. Preheat plateau results using surface grains and slices show that significant thermal transfer in naturally bleached samples can be avoided by keeping preheat temperatures low. Equivalent doses from surface K-feldspar grains were highly scattered and much larger than expected (0.02 Gy to >100 Gy), while solid surface slices gave more reproducible small doses (mean = 0.17±0.02 Gy, n = 32). Neither crushing nor partial bleaching were found to be responsible for the large scattered doses from grains, nor did the inevitable contribution from Na-feldspar to the signal from solid slices explain the improved reproducibility in the slices. By modelling the increase of luminescence signal with distance into the rock surface, attenuation factors were derived for two samples. These indicate that, for instance, bleaching at a depth of 2 mm into these samples occurs at about ∼28% of the rate at the surface. We conclude that it should be possible to derive meaningful burial doses of >1 Gy from such cobbles; younger samples would probably require a correction for incomplete bleaching.     

Luminescence geochronology and paleoenvironmental implications of coastal deposits of southeast Cyprus

Quaternary stratigraphy and sea level changes have been extensively investigated in many areas of the Mediterranean. However, numerical dating of coastal deposits and the associated paleoenvironmental information are limited for the coasts of Cyprus, principally based on radiometric and radiation-exposure geochronological techniques on fossils which bear a range of limitations and uncertainties. As such, optically stimulated luminescence (OSL) dating techniques are deemed to be the most suitable in direct dating of the coastal sediments of Cyprus. In the southeastern Cyprus, coastal dunes (aeolianites) now forming elongated ridges appear as morphological features running parallel to the current shoreline presenting an indicator of sea level and climate changes of great paleoenvironmental significance. We present our first chronological results for the exposed aeolianites and underlying littoral deposits formed along the southeastern coastal Cyprus ranging from 78.4 ± 9.9 to 56.2 ± 7.4 ka. The post-infrared–infrared stimulated luminescence (pIR-IRSL) revealed that dune formation took place during the marine isotope stages (MISs) 3, 4, and possibly 5a. Late Holocene reworking is proposed for a distinctively isolated dune with an age of ~1.3 ka ago. This study also showed that pIR-IRSL dating of feldspars may be a reliable alternative to quartz OSL dating when the quartz luminescence characteristics are unsuitable.     

Dating North Asian surface assemblages with ostrich eggshell: implications for palaeoecology and extirpation

East Asian ostrich (Struthio anderssoni Lowe) was thought to have become extinct sometime in the Late Pleistocene. Petroglyphs portray ostrich with Pleistocene animals, and ostrich eggshell (OES) fragments and ornaments from Holocene sites were considered to be older fossils. Here we summarize previous radiometric dates for ostrich eggshell (OES) and present 15 new calibrated accelerator mass spectrometry (AMS) dates, indicating that ostrich survived in Mongolia and northern China until at least 8.9 ka BP. The dates in our sample population suggest a correlation between Struthio and warm steppe environments, with extirpation probably related to essential changes in Holocene steppe ecosystems including human expansion. This study assesses the usefulness of Asian OES for archaeological dating by AMS, constrains the date of Asian ostrich extirpation, and investigates palaeoenvironmental implications of ostrich survival and extinction.     

COMPOSITIONAL INHOMOGENEITY OF SEDIMENTS AND ITS POTENTIAL EFFECTS ON DOSE RATE ESTIMATION FOR ELECTRON SPIN RESONANCE DATING OF TOOTH ENAMEL

We present results of particle size and radioactivity analyses of sediment samples collected from five sites with different burial environments. The uranium, thorium and potassium concentrations in the five sample sets are shown to vary with particle size. The potential effects of the observed size-dependent variations on electron spin resonance (ESR) dating of tooth enamel are assessed using two hypothetical models. Our results show that any bias to relatively fine fractions could result in a significant overestimation of the total environmental dose rate, leading to an underestimation of the calculated ESR age.     

New datings of Amudian layers at Qesem Cave (Israel): results of TL applied to burnt flints and ESR/U-series to teeth

Because only a few radiometric data are actually available, the chronology of the Amudian – a blade-dominated industry of the Acheulo-Yabrudian Cultural Complex (AYCC) of the late Lower Paleolithic in the Levant – is still not well constrained. Qesem Cave offers the opportunity to enhance our knowledge of the chronological position of this industry which is unique to the Levant. The Qesem Amudian bearing layers yielded also human remains showing affinities with those of modern populations recovered in the Middle Paleolithic sites of Skhul and Qafzeh. The results presented here are the first attempt to apply the TL and ESR/U-series dating methods at this site and these methods yielded results which are generally in agreement. They support a time interval of hominid-bearing occupation of the areas of the cave where Amudian lithic artifacts were recovered during MIS 8 and likely 9 for the Deep Pit Area, and during MIS 8 and possibly 7 for the Upper part of the sequence (Square K/10 and the Eastern Microfauna-Bearing Area). An older occupation of the cave is also conceivable on the base of two dating results (MIS 11).     

ESR and AMS-based 14C Dating of Mousterian Levels at Mujina Pećina,Dalmatia, Croatia

This paper presents the first chronometric dates for sediments that contain a Mousterian industry in Dalmatia (south Croatia). Electron spin resonance (ESR) dating was conducted on two teeth from the Mousterian level E1 at the site of Mujina Pećina. Additionally five bone and one charcoal sample from five different strata of origin at this site were dated by accelerator mass spectrometry (AMS). Assuming 30% moisture for both the gamma and beta dose rate calculations, the mean LU ESR age estimate is 44±5 ka for level E1, which is statistically indistinguishable from the mean EU ESR age estimate of 40±7 ka. A single, uncalibrated ¹⁴C age from the E1/E2 interface yielded an age estimate of 45,170 +2780/−2060 years bp while the mean of the five samples from overlying Mousterian levels is 39±3 ka. The true (calibrated) age of this mean is about 42 ka, which means that the entire stratigraphic profile in Mujina Pećina apparently was very rapidly deposited, and that the ESR age, regardless of uptake model is in good agreement with the calibrated ¹⁴C mean age. Temporally, Mujina Pećina overlaps with Pontinian Mousterian sites in west-central Italy and Vindija level G3 from northwestern Croatia. However, there are notable differences between the Mousterian industry from Mujina Pećina and these other sites. Collectively, the Croatian sites yield important evidence on the adaptation of European Mousterian people.     

ESR Dating of Micoquian Industry and Neanderthal Remains at K?lna Cave, Czech Republic

Electron spin resonance (ESR) and mass spectrometric U-series dating has been carried out on teeth recovered from K?lna cave during the excavations of 1961–76. Linear and early uptake (LU and EU) age estimates are similar due to low internal U content of the teeth. In general, ESR ages decrease upward in the section, but teeth from stone-rich (“lumpy”) layers give anomalously young ages, due to uneven dose-rate distribution. Elephant molars also give anomalously low ages, apparently due to self-absorption of gamma dose. Disregarding anomalous data, earliest appearance of Micoquian lithics and last occurrence ofDicerorhinus kirchbergensisin layer 9b is dated to 69±8 ka, which places them near the oxygen isotope stage (OIS) 5a/4 boundary. Neanderthal remains and the latest occurrence of Micoquian lithics in level 7a are dated to 50±5 ka, in good agreement with an uncalibrated radiocarbon date for this level of about 45 ka. The interstadial character of the fauna of this level also agrees with its date which places it in OIS 3. We also report that three stadial/interstadial cycles recognized in the lithological, faunal and palynological record of levels 9b through 7a at Kölna occurred during the timespan from about 70 to 50 ka.     

The archaeology and paleoenvironment of an Upper Pleistocene hyena den: An integrated approach

Data of high resolution for reconstructions of archaeological site formation processes can be obtained only by the use of precise excavation methods and comprehensive recovery techniques using fine-mesh water screening, followed by meticulous sorting and quantitative studies of all the small organic components from the screens. These methods are generally used at human occupation sites, but are not often employed at paleontological or mixed human-carnivore sites. At the site of Bois Roche, an Upper Pleistocene hyena den, we have used these meticulous recovery techniques in combination with absolute dating, geoarchaeological observations, taphonomic analyses, studies of microvertebrates and pollen analysis. Correlation of the site environmental data from pollen and microvertebrate assemblages with the vegetation record of a deep-sea core taken in the Bay of Biscay have allowed us to constrain the ages provided by ESR dating of bovid teeth and to reconstruct the physical environment of the site with a degree of confidence rarely achieved by the use of fossil remains from archaeological sites alone.