U–Pb dating of calcite–aragonite layers in speleothems from hominin sites in South Africa by MC-ICP-MS

Speleothems are found in association with hominin fossil-bearing cave deposits in South Africa and can be used to provide valuable chronological constraints. Such material is generally too old for U–Th dating and, although U–Pb geochronology presents a suitable alternative, bulk U concentrations are typically too low (<0.05 μg/g) to provide useful ages. For this reason, we used a simple non-invasive beta-scanner imaging screening step to identify U-rich (≥1 μg/g) domains that could be analyzed with MC-ICP-MS techniques to provide U–Pb ages. We demonstrate the technique using samples from Sterkfontein cave that exhibit infrequent <1 cm-thick layers with U concentrations ≥1 μg/g. Relict aragonite needles are found exclusively in these U-rich layers. We analyzed material from the same flowstone suite as Walker et al. (2006) and obtained a U–Pb age of ～2.3 Ma that agrees well with their estimate of 2.24 ± 0.09 Ma. We also obtained similar U–Pb (0.164 ± 0.026 to 0.200 ± 0.052 Ma) and U–Th (0.148 ± 0.003 Ma) ages for another sample exhibiting U-rich layers. We recognize that open-system behaviour during the partial transformation of aragonite to calcite is a potential problem and argue, on the basis of geochemistry and age consistencies, that recrystallization took place rapidly after speleothem formation and did not significantly affect the U–Pb ages.     

ESR dating of Pleistocene archaeological localities of the Nihewan Basin,North China – Preliminary results

The well-developed, late Cenozoic Nihewan Beds in northern China are amongst the most famous and well-preserved Quaternary strata in East Asia. The Nihewan Basin is also well-known for its mammalian fossils and stone artifacts, which document early human settlements in high northern latitudes (around 40°N). It is a key geological place to study palaeoenvironments and ancient human activities due to the excellent age-control of the formation by palaeomagnetism. In the present paper, the sediments of two Paleolithic sites were dated using the ESR signals of the titanium center in quartz. In order to check the reliability of our analytical procedures, a reference sample collected near the Brunhes/Matuyama (B/M) boundary at the Donggutuo site was firstly analyzed, yielding an age of 750 ± 88 ka. Then, three samples collected from the Dongpo site were analyzed by the same procedures. Our ESR results indicate that the age of the Dongpo cultural layer ranges between 304 ± 12 ka and 333 ± 23 ka, with an average of approximately 321 ± 15 ka.     

OSL dating of individual quartz ‘supergrains’ from the Ancient Middle Palaeolithic site of Cuesta de la Bajada,Spain

Dose saturation represents a fundamental limitation for obtaining finite optically stimulated luminescence (OSL) quartz ages over Middle Pleistocene timescales. Single-grain OSL studies typically reveal significant intra- and inter-sample variability in quartz dose saturation properties at the individual grain level. This enhanced variability may offer the potential to obtain extended-range chronologies exceeding the traditional upper age limits of multiple-grain OSL dating. However, there have been relatively few detailed assessments of single-grain OSL properties over high dose ranges. In this study we investigate extended-range single-grain OSL dating potential at Cuesta de la Bajada, one of the most important Ancient Middle Palaeolithic sites in the Iberian Peninsula. The quartz samples from this site exhibit exceptional dose saturation properties and contain significant populations of individual ‘supergrains’ with bright OSL signals, very high characteristic saturation dose (D₀) limits of 200 to >600 Gy, and dose-response curves that closely conform to single saturating exponential functions. Assessments of OSL signal composition and the ability to successfully recover a known laboratory dose of 470 Gy support the potential for obtaining high equivalent dose (D_e) values with reasonable fitting uncertainties. A series of novel sensitivity tests are used to assess potential biases in supergrain D_e estimation over high dose ranges related to (i) thermally transferred signal contributions, (ii) choice of dose-response curve fitting function, and (iii) insufficient dose saturation properties of individual grains. The single-grain D_e values obtained using the standard quality assurance criteria and novel sensitivity tests are consistent at 2σ, and are in agreement with quartz Ti-centre ages obtained on two of three paired electron spin resonance (ESR) samples collected from Cuesta de la Bajada. These comparisons support the suitability of our single-grain OSL results and suggest there may be good potential for using quartz supergrains to establish extended-range chronologies at some Middle Pleistocene sites. Comparisons with other single-grain OSL studies across the Iberian central plains suggest that favourable dose saturation properties may be influenced by regional-scale geological controls. The importance of undertaking single-grain OSL dating at Cuesta de la Bajada is also demonstrated by the results of synthetic aliquot experiments, which reveal multiple-grain age offsets of 60–170 ka when unsuitable grain types are inadvertently included in the final age calculations. The single-grain OSL results indicate that the main archaeological horizon at Cuesta de la Bajada (unit CB3) accumulated between 264 ± 22 and 293 ± 24 ka. These ages are consistent with the chronologies of other key early Middle Palaeolithic sites in the region (Ambrona AS6 and Gran Dolina TD10) and indicate that the Ancient Middle Palaeolithic techno-complex likely spread across Iberia from at least Marine Isotope Stage 9 onwards.     

Age models for long lacustrine sediment records using multiple dating approaches – An example from Lake Bosumtwi,Ghana

The continuous 300-m long drill cores obtained from Lake Bosumtwi, Ghana represent one of the longest, continuous lacustrine sequences obtained from an extant lake, and contain an unprecedented record of late Quaternary climate change in West Africa. However, one of the main challenges associated with generating long paleoclimate time series from terrestrial records such as this is the development of accurate age-depth relationships because unlike marine records, lacustrine sequences cannot be tuned to global ice volume records via δ¹⁸O stratigraphy. The Lake Bosumtwi record thus offers an excellent case study for examining the potential and the challenges associated with different geochronological techniques in lacustrine systems. In the present study, we use a combination of radiocarbon, optically stimulated luminescence and U-series dating and paleomagnetic excursions to generate a chronology for the upper ca. 150 ka of sedimentation at Lake Bosumtwi and employ a Bayesian approach to generate a continuous age-depth relationship. The resultant chronology is then used to test the effectiveness of tuning of an environmental magnetic proxy for dust against a well-dated record of high latitude dust. Our approach highlights the advantages of using multiple dating approaches, and the dangers of relying on too few age constraints when dating long sedimentary sequences. However, the excellent agreement between the different approaches over most of the record suggest that well-constrained age-depth models for long sedimentary sequences can be produced using this combination of approaches. Furthermore, our data provide support for extending the chronology beyond the limit of radiocarbon, U-series and OSL in the future using paleomagnetic excursions/reversals and tuning against well-dated high latitude paleoclimate records.     

U–Th radioactive disequilibrium and ESR dating of a barite-containing sulfide crust from South Mariana Trough

A block of sulfide crust collected from an active hydrothermal mound in an Archaean site (12°56.4′N, 143°37.9′E; depth ca. 3000 m) of the South Mariana Trough was dated using both ²³⁰Th/²³⁴U disequilibrium and electron spin resonance (ESR) methods to establish the growth duration. Eight subsamples from the sulfide crust were separated further into magnetic and non-magnetic fractions using a Franz isodynamic separator. Thirteen sulfide samples, soluble in nitric acid, yielded ²³⁰Th/²³⁴U ages of 0.3–2.2 ka. The magnetic fractions had significantly lower Th/U ratios, which enabled age determinations as precise as ±2% (2σ). The age distribution obtained for the section of sulfide crust analyzed is consistent with deposition of sulfide minerals from the upper surface of the crust to the inner side. The ²³⁰Th/²³⁴U ages of the sulfide minerals were compared with ESR ages of barites separated from 12 subsamples of the same sulfide crust. ESR ages of 0.27–1.3 ka show a spatial pattern broadly resembling that observed in ²³⁰Th/²³⁴U dating method. While there are some significant offsets, these results illustrate the potential of the two methods for use in investigation of the evolutional history of a hydrothermal system.     

OSL dating of fine and coarse quartz from a Palaeolithic sequence on the Bistrița Valley (Northeastern Romania)

Previous works focused on optically stimulated luminescence dating of quartz extracted from Romanian and Serbian loess reported significant discrepancies between ages obtained on fine (4–11 μm) and coarse (63–90 μm) quartz. The present study is directed at expanding these investigations. The SAR-OSL and double SAR-OSL protocols are applied on quartz of different grain sizes belonging to 9 samples extracted from a newly identified archaeological site at Bistricioara-Lutărie III on the Bistrița Valley (NE Romania). Radiocarbon ages are also obtained for the 3 uppermost cultural layers hosted in the loess-like deposit.Discrepant ages are obtained between fine (4–11 μm) and coarse (63–90 and 90–200 μm, respectively) quartz for equivalent doses higher than ∼80–100 Gy. However, a very good agreement is achieved for the youngest sample, with an age of ∼8 ka (with a D_e of 38 Gy for fine and 35 Gy for coarse grains, respectively). The comparison with independent control provided by radiocarbon dating suggests better agreement of ages calculated for coarse quartz. Our results are once again proof that concerns should be raised regarding the reliability of the equivalent doses obtained on quartz samples for which the laboratory dose response cannot be fitted by a single saturating exponential function. Further systematic investigations are required regarding the very different saturation characteristics of fine and coarse grained quartz.     

High-resolution optical dating of Late Holocene storm surge deposits – a showcase from Schokland (Noordoostpolder,the Netherlands)

Storm surges have a major impact on land use and human habitation in coastal regions. Our knowledge of this impact can be improved by correlating long-term historical storm records with sedimentary evidence of storm surges, but so far few studies have applied such an approach. Here we apply, for the first time, state-of-the-art optically stimulating luminescence (OSL) methods to obtain high-resolution age information on a sequence of Late Holocene storm surge deposits. By combining this chronological framework of storm surges with other reconstruction methods, we investigate the storm surge impact on the former island Schokland, located in a former inlet of the North Sea (central Netherlands).During the Late Holocene, Schokland transformed from a peat area that gradually inundated (~800 CE) via an island in a marginal marine environment (~1600 CE) to a land-locked island in the reclaimed Province of Flevoland (1942 CE). These transitions are recorded in the sediment archive of the island, consisting of silty clay with sandy intervals deposited during storm surges. A series of ten quartz OSL ages, obtained using best-practice methods to deal with incomplete resetting of the OSL signal and dose rate heterogeneity, reveal two periods of storm surge deposition, around 1600 CE and between 1742 and 1822 CE. Historical sources indicate that major storm surges hit Schokland during these periods. Laboratory analyses (thermogravimetry, grain-size, foraminifera, bivalves and ostracods) corroborates the existence of the two sets of storm surge deposits within the clay sequence. Our study sets a benchmark for obtaining robust depositional age constraints from storm surge sediments, and demonstrates the great potential of modern OSL methods to contribute to improved assessment of storm surge risk. © 2018 John Wiley & Sons, Ltd.     

Luminescence properties and optically (post-IR blue-light) stimulated luminescence dating of limnic sediments from northern Lake Malawi – Chances and limitations

Affected by the shifting Intertropical Convergence Zone, Lake Malawi holds an outstanding limnic sediment archive storing palaeo-environmental information of a climatically highly responsive landscape in the East African Rift Valley. Reliable chronological data are essential to interpret the lake-bottom sediments and optically stimulated luminescence (OSL) dating is an important method to build up the chronology. We report on material-property studies and OSL-dating results for polymineral fine grains extracted from piston cores obtained from the northern basin of Lake Malawi during the 1998 campaign of the International Decade of the East African Lakes (IDEAL). OSL-dating is based on a post-IR blue (pIRB) light stimulation single aliquot regeneration (SAR) protocol. Our results support earlier publications demonstrating the general applicability of OSL-dating on Lake Malawi sediments of Holocene and late Pleistocene age. However, the study also shows that dose rate estimations imply major challenges which need to be investigated in more detail to improve future OSL-dating results.     

Zircon U–Pb dating of Pubei granite and strontium isotope from sphalerite of the Xinhua Pb–Zn–(Ag) deposit,Yunkai Area of Guangxi Province,South China

The Yunkai Area is located at the southern South China Block and is part of the Qinzhou Bay-Hangzhou Bay Metallogenic Belt, which is a famous polymetallic mineralization belt. The Xinhua Pb–Zn–(Ag)deposit is located in the western part of Yunkai Area, with an abundance of Pubei batholiths. Zircon U–Pb geochronology of Pubei batholiths shows that crystallization age ranges from 251.9 ± 2.2 to 244.3 ± 1.8 Ma, thus belonging to Indosinian orogeny. Geochemistry and Sr isotopic compositions of the Pubei batholiths show that it is derived from the partial melting of large scale crustal melting during the stage of exhumation and uplifting of the lower-middle crust. In addition, strontium isotope of sphalerite from the Xinhua Pb–Zn–(Ag) deposit, has limited ranges in ~(87)Rb/~(86)Sr and ~(87)Sr/~(86)Sr, ranging from 0.4077 to 1.0449, and 0.718720 to 0.725245, respectively. The initial ~(87)Sr/~(86)Sr ratios of sphalerite ranges between 0.718720 and 0.725245, which is higher than that of upper continental crust and lower than that of the Pubei batholiths, illustrating the fluid might be derived from the mixing of Pubei pluton and upper continental crust.