The <i>μ</i>Dose system: determination of environmental dose rates by combined alpha and beta counting – performance tests and practical experiences

The μDose system is a recently developed analytical instrument applying a combined α- and β-sensitive scintillation technique for determining the radioactivity arising from the decay chains of 235U, 238U and 232Th as well as from the decay of 40K. The device was designed to meet the particular requirements of trapped charge dating methods and allows the assessment of environmental (i.e. low) levels of natural radionuclides. The μDose system was developed as a piece of low-cost laboratory equipment, but a systematic test of its performance is still pending. For the first time, we present results from a comprehensive performance test based on an inter-laboratory comparison. We compare the results obtained with μDose measurements with those from thick source alpha counting (TSAC), inductively coupled plasma optical emission spectrometry (ICP-OES) and low-level high-resolution gamma spectrometry (HRGS) applied in five participating laboratories. In addition, the reproducibility and accuracy of μDose measurements were tested on certified reference materials distributed by the International Atomic Energy Agency (IAEA; RGU-1, RGTh-1 and RGK-1) and on two loess standards (Nussy and Volkegem) frequently used in trapped charge dating studies. We compare μDose-based results for a total of 47 sediment samples with results previously obtained for these materials by well-established methods of dose rate determination. The investigated natural samples cover a great variety of environments, including fluvial, aeolian, littoral, colluvial and (geo-)archaeological sites originating from high and low mountain regions as well as from lowlands in tropical areas, drylands and mid-latitude zones of Europe, Africa, Australia, Central Asia and the Americas. Our results suggest the μDose system's capability of assessing low-level radionuclide contents with very good accuracy and precision comparable to well-established dosimetry methods. Based on the results of our comparative study and with respect to the practical experiences gained so far, the μDose system appears to be a promising tool for trapped charge dating studies.

Deconvolution of fission-track length distributions and its application to dating and separating pre- and post-depositional components

To enable the separation of pre- and postdepositional components of the length distribution of (partially annealed) horizontal confined fission tracks, the length distribution is corrected by deconvolution. Probabilistic least-squares inversion corrects natural track length histograms for observational biases, considering the variance in data, modelization, and prior information. The corrected histogram is validated by its variance–covariance matrix. It is considered that horizontal track data can exist with or without measurements of angles to the c axis. In the latter case, 3D histograms are introduced as an alternative to histograms of c-axis-projected track lengths. Thermal history modelling of samples is not necessary for the calculation of track age distributions of corrected tracks. In an example, the age equations are applied to apatites with predepositional (inherited) tracks in order to extract the postdepositional track length histogram. Fission tracks generated before deposition in detrital apatite crystals are mixed with post-depositional tracks. This complicates the calculation of the post-sedimentary thermal history, as the grains have experienced different thermal histories prior to deposition. Thereafter, the grains share a common thermal history. Thus, the extracted post-depositional histogram without inherited tracks may be used for thermal history calculation.

Deformation recorded in polyhalite from evaporite detachments revealed by ⁴⁰Ar ∕ ³⁹Ar dating

The Salt Range Formation is an extensive evaporite sequence in northern Pakistan that has acted as the primary detachment accommodating Himalayan orogenic deformation from the north. This rheologically weak formation forms a mylonite in the Khewra Mine, where it accommodates approximately 40 km displacement and is comprised of intercalated halite and potash salts and gypsiferous marls. Polyhalite [K2Ca2Mg(SO4)4⚫2H2O] grains taken from potash marl and crystalline halite samples are used as geochronometers to date the formation and identify the closure temperature of the mineral polyhalite using the 40Ar/39Ar step-heating laser and furnace methods. The diffusion characteristics measured for two samples of polyhalite are diffusivity (D0), activation energy (Ea), and %39Ar. These values correspond to a closure temperature of ca. 254 and 277 ∘C for a cooling rate of 10 ∘C Myr−1. 40Ar/39Ar age results for both samples did not return any reliable crystallisation age. This is not unexpected as polyhalite is prone to 40Ar* diffusion loss and the evaporites have experienced numerous phases of deformation resetting the closed K/Ar system. An oldest minimum heating step age of ∼514 Ma from sample 06-3.1 corresponds relatively well to the established early Cambrian age of the formation. Samples 05-P2 and 05-W2 have measured step ages and represent a deformation event that partially reset the K/Ar system based on oldest significant ages between ca. 381 and 415 Ma. We interpret the youngest measured step ages, between ca. 286 and 292 Ma, to represent the maximum age of deformation-induced recrystallisation. Both the youngest and oldest measured step ages for samples 05-P2 and 05-W2 occur within the time of a major unconformity in the area. These dates may reflect partial resetting of the K/Ar system from meteoric water infiltration and recrystallisation during this non-depositional time. Otherwise, they may result from mixing of Ar derived by radiogenic decay after Cambrian precipitation with partially reset Ar from pervasive Cenozoic deformation and physical recrystallisation.

Erosion rates in a wet, temperate climate derived from rock luminescence techniques

A new luminescence erosion meter has huge potential for inferring erosion rates on sub-millennial scales for both steady and transient states of erosion, which is not currently possible with any existing techniques capable of measuring erosion. This study applies new rock luminescence techniques to a well-constrained scenario provided by the Beinn Alligin rock avalanche, NW Scotland. Boulders in this deposit are lithologically consistent and have known cosmogenic nuclide ages and independently derived Holocene erosion rates. We find that luminescence-derived exposure ages for the Beinn Alligin rock avalanche were an order of magnitude younger than existing cosmogenic nuclide exposure ages, suggestive of high erosion rates (as supported by field evidence of quartz grain protrusions on the rock surfaces). Erosion rates determined by luminescence were consistent with independently derived rates measured from boulder edge roundness. Inversion modelling indicates a transient state of erosion reflecting the stochastic nature of erosional processes over the last ∼4.5 kyr in the wet, temperate climate of NW Scotland. Erosion was likely modulated by known fluctuations in moisture availability and to a lesser extent temperature, which controlled the extent of chemical weathering of these highly lithified rocks prior to erosion. The use of a multi-elevated temperature, post-infra-red, infra-red stimulated luminescence (MET-pIRIR) protocol (50, 150 and 225 ∘C) was advantageous as it identified samples with complexities that would not have been observed using only the standard infra-red stimulated luminescence (IRSL) signal measured at 50 ∘C, such as that introduced by within-sample variability (e.g. surficial coatings). This study demonstrates that the luminescence erosion meter can infer accurate erosion rates on sub-millennial scales and identify transient states of erosion (i.e. stochastic processes) in agreement with independently derived erosion rates for the same deposit.

Cosmogenic nuclide exposure age scatter records glacial history and processes in McMurdo Sound, Antarctica

The preservation of cosmogenic nuclides that accumulated during periods of prior exposure but were not subsequently removed by erosion or radioactive decay complicates interpretation of exposure, erosion, and burial ages used for a variety of geomorphological applications. In glacial settings, cold-based, non-erosive glacier ice may fail to remove inventories of inherited nuclides in glacially transported material. As a result, individual exposure ages can vary widely across a single landform (e.g., moraine) and exceed the expected or true depositional age. The surface processes that contribute to inheritance remain poorly understood, thus limiting interpretations of cosmogenic nuclide datasets in glacial environments. Here, we present a compilation of new and previously published exposure ages of multiple lithologies in local Last Glacial Maximum (LGM) and older Pleistocene glacial sediments in the McMurdo Sound region of Antarctica. Unlike most Antarctic exposure chronologies, we are able to compare exposure ages of local LGM sediments directly against an independent radiocarbon chronology of fossil algae from the same sedimentary unit that brackets the age of the local LGM between 12.3 and 19.6 ka. Cosmogenic exposure ages vary by lithology, suggesting that bedrock source and surface processes prior to, during, and after glacial entrainment explain scatter. 10Be exposure ages of quartz in granite, sourced from the base of the stratigraphic section in the Transantarctic Mountains, are scattered but young, suggesting that clasts entrained by sub-glacial plucking can generate reasonable apparent exposure ages. 3He exposure ages of pyroxene in Ferrar Dolerite, which crops out above outlet glaciers in the Transantarctic Mountains, are older, which suggests that clasts initially exposed on cliff faces and glacially entrained by rock fall carry inherited nuclides. 3He exposure ages of olivine in basalt from local volcanic bedrock in the McMurdo Sound region contain many excessively old ages but also have a bimodal distribution with peak probabilities that slightly pre-date and post-date the local LGM; this suggests that glacial clasts from local bedrock record local landscape exposure. With the magnitude and geological processes contributing to age scatter in mind, we examine exposure ages of older glacial sediments deposited by the most extensive ice sheet to inundate McMurdo Sound during the Pleistocene. These results underscore how surface processes operating in the Transantarctic Mountains are expressed in the cosmogenic nuclide inventories held in Antarctic glacial sediments.

TephraNZ: a major- and trace-element reference dataset for glass-shard analyses from prominent Quaternary rhyolitic tephras in New Zealand and implications for correlation

Although analyses of tephra-derived glass shards have been undertaken in New Zealand for nearly four decades (pioneered by Paul Froggatt), our study is the first to systematically develop a formal, comprehensive, open-access reference dataset of glass-shard compositions for New Zealand tephras. These data will provide an important reference tool for future studies to identify and correlate tephra deposits and for associated petrological and magma-related studies within New Zealand and beyond. Here we present the foundation dataset for TephraNZ, an open-access reference dataset for selected tephra deposits in New Zealand. Prominent, rhyolitic, tephra deposits from the Quaternary were identified, with sample collection targeting original type sites or reference locations where the tephra's identification is unequivocally known based on independent dating and/or mineralogical techniques. Glass shards were extracted from the tephra deposits, and major- and trace-element geochemical compositions were determined. We discuss in detail the data reduction process used to obtain the results and propose that future studies follow a similar protocol in order to gain comparable data. The dataset contains analyses of glass shards from 23 proximal and 27 distal tephra samples characterising 45 eruptive episodes ranging from Kaharoa (636 ± 12 cal yr BP) to the Hikuroa Pumice member (2.0 ± 0.6 Ma) from six or more caldera sources, most from the central Taupō Volcanic Zone. We report 1385 major-element analyses obtained by electron microprobe (EMPA), and 590 trace-element analyses obtained by laser ablation (LA)-ICP-MS, on individual glass shards. Using principal component analysis (PCA), Euclidean similarity coefficients, and geochemical investigation, we show that chemical compositions of glass shards from individual eruptions are commonly distinguished by major elements, especially CaO, TiO2, K2O, and FeOtt (Na2O+K2O and SiO2/K2O), but not always. For those tephras with similar glass major-element signatures, some can be distinguished using trace elements (e.g. HFSEs: Zr, Hf, Nb; LILE: Ba, Rb; REE: Eu, Tm, Dy, Y, Tb, Gd, Er, Ho, Yb, Sm) and trace-element ratios (e.g. LILE/HFSE: Ba/Th, Ba/Zr, Rb/Zr; HFSE/HREE: Zr/Y, Zr/Yb, Hf/Y; LREE/HREE: La/Yb, Ce/Yb). Geochemistry alone cannot be used to distinguish between glass shards from the following tephra groups: Taupō (Unit Y in the post-Ōruanui eruption sequence of Taupō volcano) and Waimihia (Unit S); Poronui (Unit C) and Karapiti (Unit B); Rotorua and Rerewhakaaitu; and Kawakawa/Ōruanui, and Okaia. Other characteristics, including stratigraphic relationships and age, can be used to separate and distinguish all of these otherwise-similar tephra deposits except Poronui and Karapiti. Bimodality caused by K2O variability is newly identified in Poihipi and Tahuna tephras. Using glass-shard compositions, tephra sourced from Taupō Volcanic Centre (TVC) and Mangakino Volcanic Centre (MgVC) can be separated using bivariate plots of SiO2/K2O vs. Na2O+K2O. Glass shards from tephras derived from Kapenga Volcanic Centre, Rotorua Volcanic Centre, and Whakamaru Volcanic Centre have similar major- and trace-element chemical compositions to those from the MgVC, but they can overlap with glass analyses from tephras from Taupō and Okataina volcanic centres. Specific trace elements and trace-element ratios have lower variability than the heterogeneous major-element and bimodal signatures, making them easier to fingerprint geochemically.

Confined fission-track revelation in apatite: how it works and why it matters

We present a new model for the etching and revelation of confined fission tracks in apatite based on variable along-track etching velocity, vT(x). Insights from step-etching experiments and theoretical energy loss rates of fission fragments suggest two end-member etching structures: constant-core, with a central zone of constant etching rate that then falls off toward track tips; and linear, in which etching rates fall linearly from the midpoint to the tips. From these, we construct a characterization of confined track revelation that encompasses all relevant processes, including penetration and widening of semi-tracks etching in from the polished grain surface, intersection with and expansion of confined tracks, and analyst selection of which tracks to measure and which to bypass. Both etching structures are able to fit step-etching data from five sets of paired experiments of fossil tracks and unannealed and annealed induced tracks in Durango apatite, supporting the correctness of our approach and providing a series of insights into the theory and practice of fission-track thermochronology. Etching rates for annealed induced tracks are much faster than those for unannealed induced and spontaneous tracks, impacting the relative efficiency of both confined track length and density measurements and suggesting that high-temperature laboratory annealing may induce a transformation in track cores that does not occur at geological conditions of partial annealing. The model quantifies how variation in analyst selection criteria, summarized as the ratio of along-track to bulk etching velocity at the etched track tip (vT/vB), likely plays a first-order role in the reproducibility of confined length measurements. It also accounts for and provides an estimate of the large proportion of tracks that are intersected but not measured, and it shows how length biasing is likely to be an insufficient basis for predicting the relative probability of detection of different track populations. The vT(x) model provides an approach to optimizing etching conditions, linking track length measurements across etching protocols, and discerning new information on the underlying structure of fission tracks.

Technical Note: Noble gas extraction procedure and performance of the Cologne Helix MC Plus multi-collector noble gas mass spectrometer for cosmogenic neon isotope analysis

We established a new laboratory for noble gas mass spectrometry that is dedicated to the development and application to cosmogenic nuclides at the University of Cologne (Germany). At the core of the laboratory are a state-of-the-art high-mass-resolution multicollector Helix MC Plus (Thermo Fisher Scientific) noble gas mass spectrometer and a novel custom-designed automated extraction line. The mass spectrometer is equipped with five combined Faraday multiplier collectors, with 1012 and 1013 Ω pre-amplifiers for faraday collectors. We describe the extraction line and the automated procedure for cosmogenic neon and the current performance of the experimental set-up. Performance tests were conducted using gas of atmospheric isotopic composition (our primary standard gas), as well as CREU-1 intercomparison material, containing a mixture of neon of atmospheric and cosmogenic composition. We use the results from repeated analysis of CREU-1 to assess the performance of the current experimental set-up at Cologne. The precision in determining the abundance of cosmogenic 21Ne is equal to or better than those reported for other laboratories. The absolute value we obtain for the concentration of cosmogenic 21Ne in CREU is indistinguishable from the published value.

Short communication: Inverse isochron regression for Re–Os, K–Ca and other chronometers

Conventional Re–Os isochrons are based on mass spectrometric estimates of 187Re/188Os and 187Os/188Os, which often exhibit strong error correlations that may obscure potentially important geological complexity. Using an approach that is widely accepted in 40Ar/39Ar and U–Pb geochronology, we here show that these error correlations are greatly reduced by applying a simple change of variables, using 187Os as a common denominator. Plotting 188Os/187Os vs. 187Re/187Os produces an “inverse isochron”, defining a binary mixing line between an inherited Os component whose 188Os/187Os ratio is given by the vertical intercept, and the radiogenic 187Re/187Os ratio, which corresponds to the horizontal intercept. Inverse isochrons facilitate the identification of outliers and other sources of data dispersion. They can also be applied to other geochronometers such as the K–Ca method and (with less dramatic results) the Rb–Sr, Sm–Nd and Lu–Hf methods. Conventional and inverse isochron ages are similar for precise datasets but may significantly diverge for imprecise ones. A semi-synthetic data simulation indicates that, in the latter case, the inverse isochron age is more accurate. The generalised inverse isochron method has been added to the IsoplotR toolbox for geochronology, which automatically converts conventional isochron ratios into inverse ratios, and vice versa.

Exposure dating of detrital magnetite using ³He enabled by microCT and calibration of the cosmogenic ³He production rate in magnetite

We test whether X-ray micro-computed tomography (microCT) imaging can be used as a tool for screening magnetite grains to improve the accuracy and precision of cosmogenic 3He exposure dating. We extracted detrital magnetite from a soil developed on a fanglomerate at Whitewater, California, which was offset by the Banning strand of the San Andreas Fault. This study shows that microCT screening can distinguish between inclusion-free magnetite and magnetite with fluid or common solid inclusions. Such inclusions can produce bulk 3He concentrations that are significantly in excess of the expected spallation production. We present Li concentrations, major and trace element analyses, and estimated magnetite (U–Th) / He cooling ages of samples in order to model the contribution from fissiogenic, nucleogenic, and cosmogenic thermal neutron production of 3He. We show that mineral inclusions in magnetite can produce 3He concentrations of up to 4 times that of the spallation component, leading to erroneous exposure ages. Therefore, grains with inclusions must be avoided in order to facilitate accurate and precise magnetite 3He exposure dating. Around 30 % of all grains were found to be without inclusions, as detectable by microCT, with the largest proportion of suitable grains in the grain size range of 400–800 µm. While grains with inclusions have 3He concentrations far in excess of the values expected from existing 10Be and 26Al data in quartz at the Whitewater site, magnetite grains without inclusions have concentrations close to the predicted depth profile. We measured 3He concentrations in aliquots without inclusions and corrected them for Li-produced components. By comparing these data to the known exposure age of 53.5 ± 2.2 ka, we calibrate a production rate for magnetite 3He at sea level and high latitude (SLHL) of 116 ± 13 at g−1 a−1. We suggest that this microCT screening approach can be used to improve the quality of cosmogenic 3He measurements of magnetite and other opaque mineral phases for exposure age and detrital studies.