Exploring IRSL50 fading variability in bedrock feldspars and implications for OSL thermochronometry

Optically Stimulated Luminescence (OSL) is a well-established Quaternary dating method, which has recently been adapted to application in low-temperature thermochronometry. The Infra-Red Stimulated Luminescence (IRSL) of feldspar, which so far is the most promising target signal in thermochronometry, is unfortunately prone to anomalous fading. The fading of feldspar IRSL is at times not only challenging to measure, but also laborious to incorporate within luminescence growth models. Quantification of IRSL fading is therefore a crucial step in OSL thermochronometry, raising questions regarding (i) reproducibility and reliability of laboratory measurements of fading, as well as (ii) the applicability of existing fading models to quantitatively predict the level of IRSL field saturation in nature. Here we investigate the natural luminescence signal and anomalous fading of IRSL measured at 50 °C (IRSL₅₀) in 32 bedrock samples collected from a variety of lithologies and exhumation settings (Alaska and Norway). We report a large span of IRSL₅₀ fading rates between samples (g_2days ranging from ∼0.5 to ∼45%/decade), which further demonstrates (i) a good reproducibility between two common fading measurement protocols, and (ii) the ability of tunnelling models to predict the level of feldspar IRSL₅₀ field saturation in nature. We observe higher IRSL₅₀ fading in feldspar with increasing Ca content, although other factors cannot be dismissed at present. Finally, our dataset confirms that the applicability of feldspar IRSL₅₀ in OSL thermochronometry is limited to rapidly-exhuming settings or warm subsurface environments.     

Luminescence dating of K-feldspar from sediments: A protocol without anomalous fading correction

A protocol for optical dating of potassium-rich feldspar (K-feldspar) is proposed. It utilizes the infrared stimulated luminescence (IRSL) signal measured by progressively increasing the stimulation temperature from 50 to 250 °C in step of 50 °C, so-called multi-elevated-temperature post-IR IRSL (MET-pIRIR) measurements. Negligible anomalous fading was observed for the MET-pIRIR signals obtained at 200 and 250 °C. This was supported by equivalent dose (D_e) measurements using the IRSL and MET-pIRIR signals. The D_e values increase progressively from 50 °C to 200 °C, but similar D_e values were obtained for the MET-pIRIR signal at 200 and 250 °C. Measurement of modern samples and bleached samples indicates that the MET-pIRIR signals have small residual doses less than 5 Gy equivalent to about 1–2 ka. We have tested the protocol using various sedimentary samples with different ages from different regions of China. The MET-pIR IRSL ages obtained at 200 and 250 °C are consistent with independent and/or quartz OSL ages.     

Luminescence thermochronometry of feldspar minerals: Optimisation of measurement conditions for the derivation of thermal kinetic parameters using isothermal holding experiments

Luminescence thermochronometry is sensitive to very low temperatures (below ∼120 °C), and enables the resolution of thermal histories over sub-Quaternary timescales. Here we apply a multi-elevated-temperature post-infrared infrared-stimulated luminescence (MET-pIR-IRSL) measurement protocol to feldspar minerals to extract thermal histories. These thermal histories depend on the thermal stability of the MET signal, and are based on the thermal kinetic parameters extracted from isothermal decay experiments. However, the derived thermal kinetic parameters vary with experimental conditions, specifically with the isothermal holding temperatures (ITL) used. We analyse samples with independently known thermal histories, together with synthetic thermal history samples and samples with unknown thermal histories to test the validity of thermal kinetic parameters obtained from different combinations of isothermal holding data. This approach is tested on feldspars of different mineralogies and lithologies. We find that the temperatures inferred from inverting the data change, depending both on the number and on the highest ITL temperature used for thermal kinetic parameter derivation. Analysed samples validate the MET-pIR-IRSL protocol for extracting thermal histories, and we suggest that four isothermal holding temperatures between 190 and 250 °C are used for appropriate thermal kinetic parameter derivation.     

Luminescence chronology of fossiliferous fluvial sediments along the middle Atbara River,Sudan

Fluvial sediments of the middle Atbara River Valley, eastern Sudan, contain abundant vertebrate fossils and stone tools. Previous work described two sedimentary units, the Butana Bridge Synthem (BBS) and the Khashm El Girba Synthem (KGS), with three divisions each (BBS1-3 and KGS1-3, from bottom to top, respectively). ²³⁰Th/U dating on bivalve shells suggested an age of ∼126 and ∼92 ka for the basal KGS2 and basal KGS3, respectively, and mammalian biochronology in combination with magnetostratigraphy suggested an age of late Early to early Middle Pleistocene for the underlying BBS. To establish a detailed chronology of this fluvial sedimentary sequence, we collected 17 luminescence samples from both sides of the Atbara River close to the Butana Bridge. Quartz OSL dating was applied to samples from the upper part of the profile (upper KGS2 and KGS3), but the signal reached saturation within the upper ∼10 m of the sequence. To select a suitable feldspar signal to date older samples beyond the limit of the quartz OSL, a comparison of the quartz OSL, feldspar post-IR IRSL at 225 and 290 °C, and pulsed IRSL signal at 50 °C was conducted for a sample from KGS3. The result showed that only the fading corrected pulsed IRSL yielded an age consistent with the quartz OSL, and the post-IR IRSL signals (both at 225 and 290 °C) overestimated the quartz age significantly. We therefore selected the pulsed IRSL signal to date the older deposits. The luminescence ages indicate that the entire BBS - KGS sequence was deposited between 224 ± 23 ka and <17 ± 1 ka, corresponding to marine isotope stages (MIS) 7–2, significantly revising previous conclusions.     

Thermally re-distributed IRSL (RD-IRSL): A new possibility of dating sediments near B/M boundary

This study attempted to probe a geologically more stable IR stimulated luminescence signal (IRSL) that explored so far. IRSL, probes the proximal pairs and, pIRSL measurements at elevated temperatures consume more distant pairs. We surmised that the residual IRSL after pIR-IRSL should arise from most distant pairs and hence should be more stable. A thermal stimulation after pIR-IRSL leads to redistribution of charges including distant pairs and this can be probed by further IRSL and pIRSL (post IR IRSL) measurements. This post IRSL following a thermal treatment is termed as redistributed IRSLs (RD IRSL and RD pIRSL) and contributes about 10% of total IRSL counts from a pristine sample. As expected RD, IRSLs are poor to be solar bleachable. Burial age of around 800 ka(with 30–40 %) using RD-IRSL and RD-pIRSL were comparable with the palaeomagnetic dating and were a factor of three higher than conventional pIR-IRSL, TRL, IR-RL and VSL ages.     

A test case for anomalous fading correction in IRSL dating

Infrared-stimulated luminescence (IRSL) dating of feldspars has the potential to date deposits beyond the age range of quartz optical (OSL) dating. Successful application of feldspar IRSL dating is, however, often precluded due to anomalous-fading, the tunnelling of electrons from one defect site to another. In this paper we test procedures proposed for anomalous-fading correction by comparing feldspar IRSL and quartz OSL dating results on a suite of samples from continental deposits from the southeastern Netherlands. We find that even after anomalous-fading correction IRSL ages underestimate the burial age of the deposits and argue that this may be a consequence of a dependency of anomalous fading rate on the dose rate and on the absorbed dose.     

Are feldspar SAR protocols appropriate for post-IR IRSL dating?

Recently proposed post-infrared infrared stimulated luminescence (post-IR IRSL or pIR) dating protocols have largely overcome problems associated with anomalous fading and have become increasingly important for age determination of Quaternary sediments. Here, we investigate the suitability of the proposed post-IR IRSL protocols for accurate equivalent-dose estimation on K-feldspar extracts. Our research focuses on potential sensitivity changes between the natural signal and the first test dose signal in single-aliquot regenerative dose (SAR) procedures that are not detected and thus not corrected using test-dose responses.For these investigations, we employed the Single Aliquot Regeneration and Added dose (SARA) procedure, which combines equivalent-dose estimation with a dose recovery test. Results indicated that high-temperature preheats (>260 °C for 60 s) may induce a trapping sensitivity change in IRSL signals measured at low temperature (<100 °C). As this sensitivity change cannot be detected through test dose responses in the SAR protocol, it may result in an invalid equivalent-dose estimation. However, trapping sensitivity changes were not observed after low temperature preheats (<260 °C for 60 s), nor in pIR signals measured at elevated temperature (>100 °C) after a high temperature preheat. Our results indicate that the SAR protocol is appropriate for equivalent-dose determination using elevated-temperature pIR signals (e.g. pIR at 290 °C or multiple elevated temperature pIR at 250 °C). The SAR protocol may also be appropriate for equivalent-dose determination using low temperature pIR signals, provided that the combination of preheat and measurement temperature is carefully chosen to avoid the unwanted effects of sensitivity change during the first preheat.     

Feldspar SARA IRSL dating of very low dose rate aeolian sediments from Sandwick South,Unst, Shetland

Young sediments, with low sensitivity and low dose rates, are challenging for luminescence dating. Here, we present work on the site of Sandwick South, a Norse settlement, in which these challenges were present. Field gamma dose rates below 0.1 mGy a⁻¹, and total dose rates of 0.4–0.5 mGy a⁻¹, combined with expected ages of less than 1 ka, resulted in a requirement for quantitative determination of equivalent doses of 0.2–0.4 Gy. The bedrock geology of the area are metagabbros, which explain both the exceptionally low dose rates and the lack of autochthonous quartz. Luminescence profiling during fieldwork revealed stratigraphically progressive OSL and IRSL signals, indicating phases in the sediments with dating potential. While laboratory characterisation recovered some quartz, its low yields and luminescence sensitivity precluded application of quartz methods. Electron microscopy confirmed the presence of feldspars, which were separated and used for IRSL Single Aliquot Regeneration Additive (SARA) analysis. Counting times for both high resolution gamma spectrometry (HRGS) and thick source beta counting (TSBC) measurements were extended by 1 order of magnitude, resulting in overall uncertainties of <6% for these low dose rates. Dose estimates were obtained using an adapted SARA protocol, incorporating long overnight preheats before first measurement, with the aim of mitigating short-term fading effects. Using these procedures, archaeologically meaningful dates were obtained from this difficult material, which are internally consistent, coherent with stratigraphy, and concordant with the radiocarbon constraints of the associated archaeological settlement. The dates demonstrate sand accumulation in the early to mid-13th century AD and also in the 18th century AD, which are contemporary with disruptive sand movements registered in other coastal regions of the Northeast Atlantic and North Sea regions. The approaches adopted here have provided solutions to the challenging conditions of this young, insensitive material and can therefore be considered to extend the range and applicability of luminescence dating methods.     

Toward the feldspar alternative for cosmogenic 10Be applications

The possibility of quantifying surface processes in mafic or volcanic environment using the potentialities offered by the in situ-produced cosmogenic nuclides, and more specifically by the in situ-produced ¹⁰Be, is often hampered by the rarity of quartz minerals in the available lithologies. As an alternative to overcome this difficulty, we explore in this work the possibility of relying on feldspar minerals rather that on quartz to perform in situ-produced ¹⁰Be measurements in such environments. Our strategy was to cross-calibrate the total production rate of ¹⁰Be in feldspar (P_10fsp) against the total production rate of ³He in pyroxene (P_3px) by measuring ³He and ¹⁰Be in cogenetic pyroxene (³He_px) and feldspar (¹⁰Be_fsp). The samples were collected from eight ignimbritic boulders, exposed from ca 120 to 600 ka at elevations ranging from 800 to 2500 m, along the preserved rock-avalanche deposits of the giant Caquilluco landslide (18°S, 70°W), Southern Peru. Along with data recently published by Blard et al. (2013a) at a close latitude (22°S) but higher elevation (ca. 4000 m), the samples yield a remarkably tight cluster of ³He_px - ¹⁰Be_fsp total production ratios whose weighted-mean is 35.6 ± 0.5 (1σ). The obtained weighted-mean ³He_px - ¹⁰Be_fsp total production ratio combined with the local ³He_py total production rate in the high tropical Andes published by Martin et al. (2017) allows to establish a total SLHL ¹⁰Be in situ-production rate in feldspar mineral (P_10fsp) of 3.57 ± 0.21 at.g⁻¹.yr⁻¹ (scaled for the LSD scaling scheme, the ERA40 atm model and the VDM of Lifton, 2016).Despite the large elevation range covered by the whole dataset (800–4300 m), no significant variation of the ³He_px - ¹⁰Be_fsp total production ratios in pyroxene and feldspar was evidenced. As an attempt to investigate the effect of the chemical composition of feldspar on the total ¹⁰Be production rate, major and trace element concentrations of the studied feldspar samples were analyzed. Unfortunately, giving the low compositional variability of our dataset, this issue is still pending.     

Testing the potential of using coarse-grain feldspars for post-IR IRSL dating of calcium sulphate-wedge growth in the Atacama Desert

The growth of vertically laminated calcium-sulphate wedges in the Atacama Desert is assumed to be driven by the interaction of moisture supply and salt dynamics in the subsurface. Geochronological data of these wedge laminations is yet sparse but indispensable to resolve wedge-growth phases and episodes of moisture supply and to use these deposits as a palaeoclimate archive in the hyperarid environment. Our pilot study presents a first approach of dating a calcium-sulphate wedge from the Atacama Desert using coarse-grain feldspar luminescence dating. Our results show a widespread and clustered equivalent-dose distribution of two wedge samples from ∼20 Gy up to saturation. Optically stimulated luminescence (OSL) of quartz revealed unsuitable properties for dating wedge deposits. Consequently, we applied post-infrared infrared stimulated luminescence (post-IR IRSL) to coarse-grained feldspars. Since feldspar single-grain measurements yielded a low number of luminescent grains, we used 1 mm aliquots as reliable single-grain proxies for genuine single-grain measurements. Data from energy-dispersive x-ray spectroscopy (EDX) showed that the feldspar single grains have large differences in their internal K content, resulting in an averaged internal K content of 3.9 ± 1.0 % for all luminescent grains. This result was subsequently used for dose rate and age calculations. Our results of equivalent-dose distributions and palaeodoses derived from the minimum age model reveal most recent wedge-growth activities at 10.6 ± 2.2 ka and 7.9 ± 1.8 ka for the two wedge samples.     

Differential weathering of feldspar and pyroxene in an arctic-alpine environment

The relative relief of adjacent plagioclase and pyroxene minerals was accurately measured on a recently-exhumed outcrop of gabbroic rocks in Leirdalen, southern Norway. Above the level of the former soil surface the feldspars protrude above the pyroxenes whereas below that level the pyroxenes are higher. Differential relief declines with increasing depth of burial down to 80 cm. On exposed surfaces the mean loss of pyroxene relative to feldspar is 103 cm³ m^?2 of rock surface. With burial down to 50 cm in an arctic-alpine Brown Soil the mean loss of feldspar relative to pyroxene is 179 cm³ m^?2. These figures represent minimum amounts of weathering over about 9000 years. The results confirm the importance of chemical weathering in arctic-alpine environments and the techniques may provide useful physical measures of degree of weathering for use in rate studies and relative-dating.     

Variations in luminescence properties of quartz and feldspar from modern fluvial sediments in three rivers

Studies of modern sediments, their sedimentology and depositional processes are important for understanding the behaviour of the luminescence characteristics of quartz and feldspar in fluvial settings. Previous studies have shown large variations in OSL characteristics of quartz from different fluvial systems, while the IRSL and pIRIR signals from K-feldspar have been understudied. We test the effects of fluvial setting on luminescence characteristics by collecting modern (<1 year old) bedload sediments down the courses of three river systems with very different hydrological characteristics, geologic contexts, and catchment lithologies. The single grain (SG) and multi-grain aliquot (MGA) OSL (quartz) and IRSL and pIRIR (K-feldspar) properties of samples were measured and compared to better understand intra- and inter-fluvial system patterns in sensitivity, bleaching, and equivalent dose (D_e) distribution skewness and kurtosis. The quartz OSL and K-feldspar IRSL and pIRIR signal sensitivities increase with downstream transport distance of sediments, confirming previous studies (quartz) and showing that IRSL signals from K-feldspar also increase in response to reworking cycles. Increasing transport distance also results in better bleaching of the OSL signal from quartz samples (MGA and SG) due to more grains being exposed to sunlight. By contrast, the IRSL and pIRIR signals retain significant residuals in all samples, though 5–15% of grains yield zero-dose D_e values and age modelling of SG data yields accurate burial dose estimates. Additionally, the skewness and kurtosis of SG OSL D_e datasets from one river increase with transport distance, with the best bleached samples exhibiting the highest skewness, thereby questioning the applicability of the skewness-value of a D_e dataset as an accurate indicator for partial-bleaching. Our data shows marked variability between (i) different river systems and (ii) the measured minerals, however consistent use of statistical models allows accurate D_e estimation in all contexts. Age modelling of SG data from K-feldspar, thus, provides a valuable tool for future fluvial research in regions where poor OSL characteristics prevent the use of quartz as a dosimeter.     

Optical dating of Holocene lake sediments: Elimination of the feldspar component in fine silt quartz samples

Optically stimulated luminescence of fine silt quartz was investigated to establish chronologies for lake sediments from the British Isles. Feldspar contamination and its potential effects on equivalent dose (D_e) determination were examined. A new feldspar contamination test based on the thermal quenching of quartz OSL and thermal assistance of feldspar OSL identified feldspar contamination in samples being treated for 20 min in 20% hydrofluoric acid. Feldspar component monitoring based on the post-IR OSL/OSL ratio was not sufficiently sensitive to monitor a feldspar component, but is a good indicator whether a standard SAR procedure can be applied successfully, despite the presence of feldspar. Based on these results we used a modified SAR protocol including a 100 s IRSL stimulation at 50 °C before OSL readout. This protocol could overcome any malign effects of feldspar even for a feldspar bearing polymineral sub-sample.     

Testing the application of quartz and feldspar luminescence dating to MIS 5 Japanese marine deposits

The applicability of both quartz and feldspar luminescence dating was tested on twenty-five samples from a marine succession now forming a coastal cliff at Oga Peninsula, Honshu Island, Japan. The quartz optically stimulated luminescence (OSL) signal shows thermal instability and linear modulated (LM)-OSL analysis revealed the dominance of a slow component. When compared with independent age control provided by two marker tephras, the quartz OSL ages grossly underestimate the depositional age. In contrast, potassium (K)-rich feldspar is a suitable dosimeter when measured using post-IR infrared stimulated luminescence (IRSL) at 225 °C (pIRIR₂₂₅). Scanning electron microscope (SEM) analyses on the feldspar extracts revealed that the grains are amorphous with small crystalline inclusions; using standard internal dose rate parameters, this would result in a too large dose rate. Dose rates were calculated using the observed grain size of 40 ± 20 μm with an assumed K concentration of 12.5 ± 0.5%. The fading corrected pIRIR₂₂₅ ages agree well with independent age control, and the sediments of the Katanishi Formation were deposited between 82 ± 6 and 170 ± 16 ka. This study demonstrates that pIRIR dating of feldspar is a powerful chronological tool for the dating of sediments of volcanic origin.     

Exploring the potential of luminescence methods for dating Alpine rock glaciers

Rock glaciers contain valuable information about the spatial and temporal distribution of permafrost. The wide distribution of these landforms in high mountains promotes them as useful archives for the deciphering of the environmental conditions during their formation and evolution. However, age constraints are needed to unravel the palaeoclimatic context of rock glaciers, but numerical dating is difficult. Here, we present a case study assessing the potential of luminescence techniques (OSL, IRSL) to date the inner sand-rich layer of active rock glaciers. We focus on the signal properties and the resetting of the signal prior to deposition by investigating single grains. While most quartz shows low signal intensities and problematic luminescence characteristics, K-feldspar exhibits much brighter and well-performing signals. Most signals from plagioclases do not show suitable properties. Luminescence signals far below saturation indicate distinct but differential bleaching. The finite mixture model was used to determine the prominent populations in the equivalent dose distributions. The luminescence ages represent travel times of grains since incorporation into the rock glacier and hence, minimum ages of rock glacier formation. Luminescence ages between 3 ka and 8 ka for three rock glaciers from the Upper Engadine and Albula region (Swiss Alps) agree well with independent age estimates from relative and semi-quantitative approaches. Therefore, luminescence seems to have the potential of revealing age constraints about processes related to the formation of rock glaciers, but further investigations are required for solving some of the problems remaining and reducing the dating uncertainties.     

Luminescence dating of marine sediments from the Sea of Japan using quartz OSL and polymineral pIRIR signals of fine grains

Luminescence dating has long been used for chronological constraints on marine sediments due to the ubiquitous dating materials (quartz and feldspar grains) and its applicability over a relatively long time range. However, one of the main difficulties in luminescence dating on marine sediments is partial bleaching, which causes age overestimations. Especially, partial bleaching is typically difficult to be detected in the fine grain fraction (FG) of marine sediments. The recently developed feldspar post-IR IRSL (pIRIR) protocol can detect non-fading signals and thus avoid feldspar signal instability. In the current study, fine grains were extracted from a gravity core in the northern Sea of Japan, and the aim is to test the feasibility of using different luminescence signals with various bleaching rates to explore the bleaching conditions of fine grain fraction in marine sediments. The results suggest that the quartz OSL signal and polymineral pIRIR signals at stimulation temperatures of 150 °C and 225 °C (pIRIR₁₅₀ and pIRIR₂₂₅) of FG were well bleached prior to deposition. The OSL ages were used to establish a chronology for this sedimentary core and the resulting age-depth relationship is self-consistent and comparable with radiocarbon dates. We conclude that different luminescence signals with various bleaching rates can be used to test the bleaching conditions of fine grain fraction in marine sediments; and the luminescence dating can be applied to marine sediments with great potential.     

Luminescence dating of scoria fall and lahar deposits from Somma–Vesuvius,Italy

Luminescence dating has been applied to scoria and lahar deposits from Somma–Vesuvius, Italy. Samples include scoria from the AD472 and 512 (or 536) eruptions and lahar deposits. In order to find a stable luminescence signal which is less affected by anomalous fading, infrared stimulated luminescence (IRSL) signals at elevated temperatures after bleaching with IR at 50 °C (termed post-IR IRSL; pIRIR) were tested at different preheat and elevated stimulation temperatures. The fading rates of both IRSL and pIRIR signals reduced dramatically with increasing preheat and pIRIR stimulation temperatures. A pIRIR signal measured at 290 °C after a preheat at 320 °C (60 s) and an IR stimulation at 50 °C (100 s) was selected to calculate the equivalent dose (D_e). The gamma spectrometry results indicate that the U-series nuclides are not in equilibrium and there is a large ²²⁶Ra excess. The dose rates and ages were calculated by assuming a ²²⁶Ra excess (over its parent ²³⁰Th) at deposition, and that this unsupported excess then decayed to the present level. The resulting luminescence ages of the two scoria samples agreed with the expected ages, and the ages of the lahar deposits indicate that they are associated with the AD1631 eruption.     

A method to evaluate the degree of bleaching of IRSL signals in feldspar: The 3ET method

In addition to dating, IRSL luminescence signals can preserve information about erosional, transport, and depositional histories of a population of grains. Knowledge of the degree of bleaching can be useful in understanding the processes that occurred during previous depositional events, as certain transport conditions result in a well bleached signal, while others result in grains retaining an inherited signal from prior events. This information can be accessed by making single-grain IRSL measurements across successively increasing temperatures, thereby isolating signals from traps of different bleachabilities.A new approach offers a way to evaluate the completeness of bleaching of a grain by testing patterns of equivalent dose (D_E) values measured at three elevated temperatures (3ET), 50, 125, and 225 °C. Consistent D_E estimates across two or more temperatures suggest a single bleaching event of sufficient duration to fully depopulate the traps involved. Incompletely bleached grains with inconsistent D_E values across temperatures will lack a 3ET “plateau.” Modes in the distribution of D_E values for fully bleached grains can suggest depositional ages, subject to assessment of fading. We developed a Python code in a Jupyter Notebook environment for data analysis and visualization to expedite processing the large data sets produced by the 3ET protocol.The 3ET protocol was tested on a radiocarbon dated sequence of playa samples from California, USA and on a set of fluvial terraces in the Marlborough region of New Zealand as part of a larger project to reconstruct regional seismic history. Where standard pIRIR apparent ages can be inconsistent or ambiguous, 3ET age estimates produce generally consistent apparent ages. Modes of 3ET plateaus can be used to infer the most recent and prior events that resulted in a sub-population of grains being fully bleached. These initial results suggest that the 3ET method can be useful to characterize both the age and degree of bleaching of depositional events.