U-series and radiocarbon cross dating of speleothems from Nerja Cave (Spain): Evidence of open system behavior. Implication for the Spanish rock art chronology

Two stalagmites from Nerja cave (Andalusia, Spain) were studied. The cave is well known because of its long human occupation from the Upper Palaeolithic to the Chalcolithic and its abundant parietal prehistoric Art. The aims of this study were twofold: i) to compare uranium/thorium (Th/U) and Carbon-14 (C) ages obtained all along the growth axis of the stalagmites in order to understand the consequences of diagenetic processes on the validity of radiometric ages; ii) as one of the stalagmites contains black layers, attributed to combustion soot, to establish when these intense hearths were used and by which culture. Th/U and C ages were coupled with mineralogical studies using FTIR (Fourier-transform infrared spectroscopy) and thin section observations. The first stalagmite (GN16-9b) displays Th/U ages in stratigraphic order, and compatible with C ages corrected for a few percent of dead carbon. Homogeneous composition of aragonitic crystals characterized by their needle-like texture is observed throughout this speleothem. For the second stalagmite (GN16-7), in contrast, Th/U ages display large significant inversions and discordant results on the upper part and at the base of the stalagmite, suggesting a possible open system behavior for this chronometer. Interestingly, C ages are in stratigraphic order all along the stalagmite and are compatible with Th/U ages only in its central part. Mineralogical studies display evidence of aragonite to calcite transformation at the top and a complex mineralogical assemblage with interlayered silicates (possibly clays) and calcitic mineralogy for the base of GN16-7. In these parts, discordant Th/U ages were measured. In the middle part of the stalagmite, however, where the fibrous aragonite is well preserved, the C and Th/U ages agree. Our data suggest that in the case of aragonite to calcite transformation as shown here, Th/U ages are biased, but C ages seem to remain accurate, as already observed in aragonitic marine bio minerals. C ages obtained are used for the chronology of the soot layer, determined here between 7900 and 5500 years Cal BP, coherent with previous analysis of charcoals in the same sector of the cave. This study highlights the importance of working with at least two chronometers when stratigraphic age verification is not possible, as is the case of some parietal CaCO thin layers used for rock art dating. Recent Th/U ages published for carbonate deposits on Spanish parietal Art are discussed in light of this demonstration.This research was funded by ANR (grant number ANR-18-CE27- 0004, ApART project) and supported by the Paris Ile-de-France Region – DIM “matérieux Anciens et Patrimoniaux” for FTIR analysis. The authors thank LMC14 staff (Laboratoire de Mesure du Carbone-14), ARTEMIS national facility, for the results obtained with the Accelerator Mass Spectroscopy method, and the PANOPLY analytical platform. This research is part of the “Proyecto General de Investigación aplicada a la conservación de Cueva de Nerja” authorised by the Junta de Andalucía and financed by the Fundación de Servicios Cueva de Nerja. The authors also wish to thank the “Instituto de Investigación Cueva de Nerja” for supporting this research. M.A.Medina-Alcaide has a Postdoctoral Fyssen Grant; the results presented in this paper are included in the PID2019-107262GB-I00 and PDC2021-121501-I00 grants funded by MCIN/AEI/10.13039/501100011033

Helium trapping in apatite damage: insights from (U-Th-Sm)/He dating of different granitoid lithologies

Apatite (U-Th-Sm)/He (AHe) thermochronometry is widely used to constrain thermal histories and rates of tectonic, exhumation, and erosion processes. However, data interpretation is often challenging, especially when the thermal history includes extended residence time in the He partial retention zone (HePRZ), with highly dispersed dates revealing the complexity of diffusion processes in natural systems. This study investigates chemical and physical factors that may have impacted He diffusion in apatite over long timescales in a context of protracted residence in the HePRZ. Nine samples from the Ploumanac'h pluton and North Tregor (Armorican Massif, France) were collected in granitoids, differing in petrography and chemisty. This area was chosen because these samples underwent a similar thermal history since ~300 Ma. We report new (U-Th Sm)/He dates, along with apatite fission-track (AFT) data, as well as lithological and chemical characterization. The results show dispersed (U-Th-Sm)/He dates, ranging from 87 ± 7 to 291 ± 23 Ma, whereas central AFT dates vary from 142 ± 6 to 199 ± 9 Ma. Current predictive models for He diffusion and fission-track annealing in apatite could not reproduce the two datasets together. However, this apparent discrepancy gives insight into the parameters influencing He diffusion at geological timescales. The data confirm that radiation damage enhances He trapping, as the AHe dates are positively correlated to effective uranium (eU) concentration. The He age dispersion for constant eU content cannot be explained just by variations in grain size or chemical composition. To explore the potential influence of recoil damage trapping behavior and annealing kinetics on AHe dates, we tested a new diffusion model from Gerin et al. (2017). Given the expected model of the thermal history provided by AFT inversion, we investigated the influence of the trapping energy on AHe dates. The AHe date variations can be explained only if the trapping energy evolves from one crystal to another, increasing with the amount of damage. For a given trapping energy, minor variations in the recoil-damage annealing rate can consistently explain most of the remaining dispersion of the AHe dates

Thermal history of the central Gotthard and Aar massifs, European Alps: Evidence for steady state, long-term exhumation

International audienceQuantifying long-term exhumation rates is a prerequisite for understanding the geodynamic evolution of orogens and their exogenic and endogenic driving forces. Here we reconstruct the exhumation history of the central Aar and Gotthard external crystalline massifs in the European Alps using apatite and zircon fission track and apatite (U-Th)/He data. Age-elevation relationships and time-temperature paths derived from thermal history modeling are interpreted to reflect nearly constant exhumation of ∼0.5 km/Ma since ∼14 Ma. A slightly accelerated rate (∼0.7 km/Ma) occurred from 16 to 14 Ma and again from 10 to 7 Ma. Faster exhumation between 16 and 14 Ma is most likely linked to indentation of the Adriatic wedge and related thrusting along the Alpine sole thrust, which, in turn, caused uplift and exhumation in the external crystalline massifs. The data suggest nearly steady, moderate exhumation rates since ∼14 Ma, regardless of major exogenic and endogenic forces such as a change to wetter climate conditions around 5 Ma or orogen-perpendicular extension initiated in Pliocene times. Recent uplift and denudation rates, interpreted to be the result of climate fluctuations and associated increase in erosional efficiency, are nearly twice this ∼0.5 km/Ma paleoexhumation rate

Toward understanding the post-collisional evolution of an orogen influenced by convergence at adjacent plate margins; Late Cretaceous-Tertiary thermotectonic history of the Apuseni Mountains

The relationship between syn- to post-collisional orogenic shortening and stresses transmitted from other neighboring plate boundaries is important for understanding the kinematics of mountain belts, but has received little attention so far. The Apuseni Mountains are an example of an orogen in the interference zone between two other subduction systems located in the external Carpathians and Dinarides. This interference is demonstrated by the results of a combined thermochronological and structural field study that quantifies the post-collisional latest Cretaceous-Tertiary evolution. The exhumation history derived from apatite fission track and (U-Th)/He thermochronology indicates that the present-day topography of the Apuseni Mountains originates mainly from latest Cretaceous times, modified by two tectonic pulses during the Paleogene. The latter are suggested by cooling ages clustering around ∼45 Ma and ∼30 Ma and the associated shortening recorded along deep-seated fault systems. Paleogene exhumation pulses are similar in magnitude (∼3.5 km) and are coeval with the final collisional phases recorded in the Dinarides and with part of the Carpathian rotation around the Moesian promontory. These newly quantified Paleogene exhumation and shortening pulses contradict the general view of tectonic quiescence, subsidence and overall sedimentation for this time interval. The Miocene collapse of the Pannonian Basin did not induce significant regional exhumation along the western Apuseni flank, nor did the subsequent Carpathian collision. This is surprising in the overall context of Pannonian Basin formation and its subsequent inversion, in which the Apuseni Mountains were previously interpreted as being significantly uplifted in both deformation stages. Copyright 2011 by the American Geophysical Union

Reply to comment on "Compositional and structural control of fission-track annealing in apatite"

International audienc

Variation in apatite fission-track length measurement: implications for thermal history modelling

Predictive thermal history modelling using apatite fission-track (FT) data is dependent on an algorithm to describe the time and temperature dependency of FT annealing which, in turn, relies on the empirical determination of FT length as a measure of the annealing process. Assessment of variation in FT length measurement is poorly described, with few comparisons between analysts and little interlaboratory standardisation. Using apatites of various compositions containing induced tracks annealed to differing degrees, this study has assessed variation in horizontal confined track-length measurement for a variety of procedural conditions. Replicate analysis by a single observer is typically within 3% but increases inversely with track length. Comparison between observers on the same samples shows significant, generally nonsystematic variation between observers; for a complex length distribution variation is ∼12%. Sources of variation are identified as: (a) variation from track revelation, including etching, track-in-track (TINT) vs. track-in-cleavage (TINCLE) measurement and use of 252Cf irradiation to produce additional etching channels; (b) bias in measurement, including equipment, analytical procedures, and sample size; and (c) observer bias, principally differences in and consistency of personal technique. 5 M HNO3 is preferred to weaker etchants: although more anisotropic, tracks are better defined, permitting more rigorous measurement, while c-axis parallel sections (where 2π/4 π geometry is better defined) are more easily identified. For all but the longest length distributions, TINCLEs are significantly longer than TINTS, with few short TINCLEs at high angles; measurement of TINCLEs effectively masks the anisotropy of annealing. 252Cf irradiation is effective in increasing the number of TINTs sampled and measured. Variation between values measured for unirradiated and Cf-irradiated aliquots does not exceed that found for a single analyst, although a slight systematic shift to longer lengths for Cf-irradiated samples is seen. As reported by other workers, track-length distributions are anisotropic, anisotropy increasing with annealing level. Track angle exerts a major influence on measured length, summing affects from annealing and etching anisotropies with observer bias. Track angle should be accommodated within the annealing algorithm. It is recommended that similar track revelation, observation and measurement conditions are used for the analysis of field samples as are used in annealing experiments, and subsequently employed in numerical models to predict thermal history. A parallel argument can be advanced for using samples of similar composition. Further, we recommend that the FT community should seek as a matter of some urgency a programme of interlaboratory comparison of track-length measurement using standard apatite samples containing artificial length distributions typifying various levels of complexity. Such comparisons would provide a more rigorous baseline for thermal history prediction in geological case studies

Modelling of the thermal history of the Carboniferous Lorraine Coal Basin: Consequences for coal bed methane

International audienceThis paper proposes a new scenario for the thermal history of the Carboniferous Lorraine Coal Basin following the tectonic model developed by Averbuch et al. (2012) and establishes some consequences for the coal bed methane (CBM) exploitation. Organic matter maturation data (Vitrinite Reflectance) determined on eleven boreholes in the eastern Lorraine have been used to characterize the Lorraine Coal Basin evolution. Paleozoic and Mesozoic overburials have been calculated using a thermal modelling software (Petromod). Results show that (1) Paleozoic erosion may be estimated at a maximum of 1200 m which represents a low amplitude event, (2) a little erosion occurred between Upper Paleozoic and Lower Mesozoic: paleotemperature offset is about 20 °C and VR data range from 0.7 (Westphalian D) to 0.5 (Lower Triassic), (3) Cretaceous cover overburial reaches a maximum of 300 m and decreases eastwards and (4) the variation of heat flows is in agreement with the compressive and extensive phases of Paleozoic and the extensive phase of Mesozoic. Consequences on the petroleum system are the following: organic matter is immature in the Jurassic and Triassic sedimentary rocks, mature (oil window) in the Permian, Stephanian and Westphalian C-D, highly mature (gas window) in Westphalian A-B-C and overmature in Namurian-Westphalian A. The high methane adsorption capacity of coal and the presence of natural fractures inside coal seams demonstrated by coal tomography allow a high CBM potential in this basin. The Lorraine Coal Basin is therefore a target for coal gas