Special Issue "Methods in Dating and Other Applications using Luminescence"

A special issue of Methods and Protocols (ISSN 2409-9279).

Deadline for manuscript submissions: closed (1 October 2019).

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A printed edition of this Special Issue is available here.

Special Issue Editor

Prof. Dr. James K. Feathers
Website
Guest Editor
University of Washington, Seattle, WA, USA
Interests: luminescence dating applications in archaeology and geology, ceramic chronology, chronology of early people in the New World, dating structures

Special Issue Information

Dear Colleagues,

The phenomenon of using luminescence to date materials began in the 1960s and 1970s in the context of dating pottery from archaeological sites. Its applications spread to sediments, both geological and archaeological, in the 1980s. Substantial developments in methods, including the introduction of optically stimulated luminescence (OSL) and infrared stimulated luminescence (IRSL) and the development of single-aliquot and single-grain techniques, over the past 30 years have made luminescence dating one of the major chronological tools in Quaternary science. Not only have the kinds of dating applications expanded, but luminescence is increasingly being used to address other kinds of questions. The latter include rates of landscape exhumation, fluvial transport dynamics, the sourcing and transport rates of sedimentary grains, soil development including mixing from bioturbation, and the incidence of wildfires. This Issue hopes to compile papers on cutting-edge methodology in dating and other applications. Potential topics include thermochronometry, sediment provenience, dating sediments older than 100,000 years or younger than 100 years, dating rock surfaces, dating archaeological structures, statistical models for single-grain equivalent dose distributions, anomalous fading in feldspars, variations in luminescence sensitivity of both quartz and feldspars, radio-fluorescence, improving dating precision, time-resolved luminescence, dose rate heterogeneity, exposure dating, modeling bioturbation, spectral applications of luminescence, novel stimulation modes, and bleaching during fluvial transport.  A younger generation of practitioners, who have earned their degrees in the last 10 years, is driving much of the methodological innovation in luminescence, and these younger scientists are particularly encouraged to submit papers.

Prof. Dr. James K. Feathers
Guest Editor

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Keywords

  • Luminescence dating methods
  • Single-grain dating
  • Quartz and Feldspar luminescence properties
  • Thermochronometry
  • Luminescence provenience
  • Fluvial dynamics
  • Soil development.

Published Papers (12 papers)

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Editorial

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Open AccessEditorial
Methods and Applications in Trapped Charge Dating
Methods Protoc. 2020, 3(1), 24; https://doi.org/10.3390/mps3010024 - 24 Mar 2020
Abstract
Trapped charge dating is a commonly used chronological tool in Earth Sciences and Archaeology. The two principle methods are luminescence dating and electron spin resonance. Both are based on stored energy produced by the absorption of natural radioactivity in common minerals such as [...] Read more.
Trapped charge dating is a commonly used chronological tool in Earth Sciences and Archaeology. The two principle methods are luminescence dating and electron spin resonance. Both are based on stored energy produced by the absorption of natural radioactivity in common minerals such as quartz and feldspars and in some biological materials such as tooth enamel. Methodological developments in the last 20 years have substantially increased accuracy and precision. This essay introduces a compilation of papers that offers a taste of recent research into both method and application. Full article

Research

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Open AccessArticle
Single Aliquot Regeneration (SAR) Optically Stimulated Luminescence Dating Protocols Using Different Grain-Sizes of Quartz: Revisiting the Chronology of Mircea Vodă Loess-Paleosol Master Section (Romania)
Methods Protoc. 2020, 3(1), 19; https://doi.org/10.3390/mps3010019 - 27 Feb 2020
Cited by 2
Abstract
The loess-paleosol archive from Mircea Vodă (Romania) represents one of the most studied sections in Europe. We are applying here the current state of the art luminescence dating protocols for revisiting the chronology of this section. Analysis were performed on fine (4–11 µm) [...] Read more.
The loess-paleosol archive from Mircea Vodă (Romania) represents one of the most studied sections in Europe. We are applying here the current state of the art luminescence dating protocols for revisiting the chronology of this section. Analysis were performed on fine (4–11 µm) and coarse (63–90 µm) quartz extracts using the single aliquot regenerative (SAR) optically stimulated luminescence (OSL) dating protocol. Laboratory generated SAR dose response curves in the high dose range (5 kGy for fine quartz and 2 kGy for coarse quartz) were investigated by employing a test dose of either 17 or 170 Gy. The results confirm the previously reported different saturation characteristics of the two quartz fractions, with no evident dependency of the equivalent dose (De) on the size of the test dose. The OSL SAR ages are discussed and compared to the previously obtained results on quartz and feldspars. The previous reports regarding the chronological discrepancy between the two quartz fractions are confirmed. However, while previous investigations on other sites concluded that this discrepancy appears only above equivalent doses of about 100 Gy, here fine grain quartz ages underestimate coarse quartz ages starting with equivalent doses as low as around 50 Gy. Full article
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Open AccessArticle
Sedimentary Dosimetry for the Saradj-Chuko Grotto: A Cave in a Lava Tube in the North-Central Caucasus, Russia
Methods Protoc. 2020, 3(1), 20; https://doi.org/10.3390/mps3010020 - 26 Feb 2020
Cited by 1
Abstract
Karst caves host most European Paleolithic sites. Near the Eurasian-Arabian Plate convergence in the Caucasus’ Lower Chegem Formation, Saradj-Chuko Grotto (SCG), a lava tube, contains 16 geoarchaeologically distinct horizons yielding modern to laminar obsidian-rich Middle Paleolithic (MP) assemblages. Since electron spin resonance (ESR) [...] Read more.
Karst caves host most European Paleolithic sites. Near the Eurasian-Arabian Plate convergence in the Caucasus’ Lower Chegem Formation, Saradj-Chuko Grotto (SCG), a lava tube, contains 16 geoarchaeologically distinct horizons yielding modern to laminar obsidian-rich Middle Paleolithic (MP) assemblages. Since electron spin resonance (ESR) can date MP teeth with 2–5% uncertainty, 40 sediment samples were analyzed by neutron activation analysis to measure volumetrically averaged sedimentary dose rates. SCG’s rhyolitic ignimbrite walls produce very acidic clay-rich conglomeratic silts that retain 16–24 wt% water today. In Layers 6A-6B, the most prolific MP layers, strongly decalcified bones hinder species identification, but large ungulates inhabited deciduous interglacial forests. Unlike in karst caves, most SCG’s layers had sedimentary U concentrations >4 ppm and Th, >12 ppm, but Layer 6B2 exceeded 20.8 ppm U, and Layer 7, >5 ppm Th. Such high concentrations emit dose rates averaging ~1.9–3.7 mGy/y, but locally up to 4.1–5.0 mGy/y. Within Layer 6, dose rate variations reflect bone occurrence, necessitating that several samples must be geochemically analyzed around each tooth to ensure age accuracy. Coupled with dentinal dose rates up to 3.7–4.5 mGy/y, SCG’s maximum datable ages likely averages ~500–800 ka. Full article
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Open AccessArticle
Optically Stimulated Luminescence Sensitivity of Quartz for Provenance Analysis
Methods Protoc. 2020, 3(1), 6; https://doi.org/10.3390/mps3010006 - 13 Jan 2020
Cited by 1
Abstract
Finding the source or provenance of quartz grains occurring in a specific location allows us to constrain their transport pathway, which is crucial information to solve diverse problems in geosciences and related fields. The optically stimulated luminescence (OSL) sensitivity (light intensity per unit [...] Read more.
Finding the source or provenance of quartz grains occurring in a specific location allows us to constrain their transport pathway, which is crucial information to solve diverse problems in geosciences and related fields. The optically stimulated luminescence (OSL) sensitivity (light intensity per unit mass per unit radiation dose) has a high capacity for discrimination of quartz sediment grains and represents a promising technique for provenance analysis. In this study, we tested the use of quartz OSL sensitivity (ultraviolet emission) measured under different preheating temperatures and with blue light stimulation at room temperature (~20 °C) for sediment provenance analysis. Quartz OSL sensitivity measured at 20 °C is positively correlated with the sensitivity of an OSL signal measured using procedures (preheat at 190 °C for 10 s, blue stimulation at 125 °C and initial 1 s of light emission) to increase the contribution of the fast OSL component, which has been successfully applied for sediment provenance analysis. The higher OSL signal intensity measured without preheating and with light stimulation at room temperature allows the use of lower given doses, thus reducing measurement time. Additionally, the OSL sensitivity measured at 20 °C in polymineral silt samples of a marine sediment core is also suitable for provenance analysis, as demonstrated by comparison with other independent proxies. OSL signals obtained through light stimulation at room temperature have thus the potential to considerably expand measurement possibilities, including in situ measurements using portable OSL readers. Full article
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Open AccessArticle
Using DosiVox to Reconstruct Radiation Transport through Complex Archaeological Environments
Methods Protoc. 2019, 2(4), 91; https://doi.org/10.3390/mps2040091 - 11 Dec 2019
Cited by 1
Abstract
The DosiVox programme is used to reconstruct radiation transport in complex depositional environments. Using two archaeological case studies from ancient Egypt, the burial environments for a selection of ceramic vessels are reconstructed using the DosiVox programme, allowing the simulation of the emission and [...] Read more.
The DosiVox programme is used to reconstruct radiation transport in complex depositional environments. Using two archaeological case studies from ancient Egypt, the burial environments for a selection of ceramic vessels are reconstructed using the DosiVox programme, allowing the simulation of the emission and transport of radiation throughout these burial environments. From this simulation we can extract the external dose rate of the archaeological samples, a measurement necessary for determine a luminescence age. We describe in detail how DosiVox can be used to best advantage at sites with complex depositional histories and highlight that DosiVox is a valuable tool in luminescence dating. This work illustrates that DosiVox is, at present, unparalleled in reconstructing a more accurate and detailed external gamma dose rate which can significantly improve upon simplistic scaled geometric models. Full article
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Open AccessArticle
Testing Luminescence Dating Methods for Small Samples from Very Young Fluvial Deposits
Methods Protoc. 2019, 2(4), 90; https://doi.org/10.3390/mps2040090 - 06 Dec 2019
Cited by 1
Abstract
The impetus behind this study is to understand the sedimentological dynamics of very young fluvial systems in the Amazon River catchment and relate these to land use change and modern analogue studies of tidal rhythmites in the geologic record. Initial quartz optically stimulated [...] Read more.
The impetus behind this study is to understand the sedimentological dynamics of very young fluvial systems in the Amazon River catchment and relate these to land use change and modern analogue studies of tidal rhythmites in the geologic record. Initial quartz optically stimulated luminescence (OSL) dating feasibility studies have concentrated on spit and bar deposits in the Rio Tapajós. Many of these features have an appearance of freshly deposited pristine sand, and these observations and information from anecdotal evidence and LandSat imagery suggest an apparent decadal stability. The characteristics of OSL from small (~5 cm) sub-samples from ~65 cm by ~2 cm diameter vertical cores are quite remarkable. Signals from medium-sized aliquots (5 mm diameter) exhibit very high specific luminescence sensitivity, have excellent dose recovery and recycling, essentially independent of preheat, and show minimal heat transfer even at the highest preheats. These characteristics enable measurement of very small signals with reasonable precision and, using modified single-aliquot regenerative-dose (SAR) approaches, equivalent doses as low as ~4 mGy can be obtained. Significant recuperation is observed for samples from two of the study sites and, in these instances, either the acceptance threshold was increased or growth curves were forced through the origin; recuperation is considered most likely to be a measurement artefact given the very small size of natural signals. Dose rates calculated from combined inductively coupled plasma mass spectrometry/inductively coupled plasma optical emission spectrometry (ICP-MS/ICP-OES) and high-resolution gamma spectrometry range from ~0.3 to 0.5 mGya−1, and OSL ages for features so far investigated range from 13 to 34 years to several 100 years. Sampled sands are rich in quartz and yields of 212–250 μm or 250–310 μm grains indicate high-resolution sampling at 1–2 cm intervals is possible. Despite the use of medium-sized aliquots to ensure the recovery of very dim natural OSL signals, these results demonstrate the potential of OSL for studying very young active fluvial processes in these settings. Full article
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Open AccessArticle
Sampling Methods for Luminescence Dating of Subsurface Deposits from Cores
Methods Protoc. 2019, 2(4), 88; https://doi.org/10.3390/mps2040088 - 22 Nov 2019
Cited by 1
Abstract
Study of subsurface deposits often requires coring or drilling to obtain samples for sedimentologic and geochemical analysis. Geochronology is a critical piece of information for stratigraphic correlation and rate calculations. Increasingly, luminescence dating is applied to sediment cores to obtain depositional ages. This [...] Read more.
Study of subsurface deposits often requires coring or drilling to obtain samples for sedimentologic and geochemical analysis. Geochronology is a critical piece of information for stratigraphic correlation and rate calculations. Increasingly, luminescence dating is applied to sediment cores to obtain depositional ages. This paper provides examples and discussion of guidelines for sampling sediment core for luminescence dating. Preferred protocols are dependent on the extraction method, sedimentology, core integrity, and storage conditions. The methods discussed include subsampling of sediment in opaque core-liners, cores without liners, previously open (split) cores, bucket auger samples, and cuttings, under red lighting conditions. Two important factors for luminescence sampling of sediment core relate to the integrity of the natural luminescence signal and the representation of the dose rate environment. The equivalent dose sample should remain light-safe such that the burial dose is not reset (zeroed) by light exposure. The sediment sampled for dose rate analyses must accurately represent all units within at least 15 cm above and below the equivalent dose sample. Where lithologic changes occur, units should be sampled individually for dose rate determination. Sediment core extraction methods vary from portable, hand-operated devices to large truck- or vessel-mounted drill rigs. We provide recommendations for luminescence sampling approaches from subsurface coring technologies and downhole samplers that span shallow to deep sample depths. Full article
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Review

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Open AccessReview
Review of the Post-IR IRSL Dating Protocols of K-Feldspar
Methods Protoc. 2020, 3(1), 7; https://doi.org/10.3390/mps3010007 - 14 Jan 2020
Cited by 3
Abstract
Compared to quartz, the infrared stimulated luminescence (IRSL) of K-feldspar saturates at higher dose, which has great potential for extending the dating limit. However, dating applications with K-feldspar has been hampered due to anomalous fading of the IRSL signal. The post-IR IRSL (pIRIR) [...] Read more.
Compared to quartz, the infrared stimulated luminescence (IRSL) of K-feldspar saturates at higher dose, which has great potential for extending the dating limit. However, dating applications with K-feldspar has been hampered due to anomalous fading of the IRSL signal. The post-IR IRSL (pIRIR) signal of K-feldspar stimulated at a higher temperature after a prior low-temperature IR stimulation has significantly lower fading rate. Different dating protocols have been proposed with the pIRIR signals and successful dating applications have been made. In this study, we review the development of various pIRIR dating protocols, and compare their performance in estimating the equivalent dose (De). Standard growth curves (SGCs) of the pIRIR signals of K-feldspar are introduced. Single-grain K-feldspar pIRIR dating is presented and the existing problems are discussed. Full article
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Other

Open AccessProtocol
Determining the Age of Terrace Formation Using Luminescence Dating—A Case of the Yellow River Terraces in the Baode Area, China
Methods Protoc. 2020, 3(1), 17; https://doi.org/10.3390/mps3010017 - 20 Feb 2020
Cited by 2
Abstract
Dating fluvial terraces has long been a challenge for geologists and geomorphologists, because terrace straths and treads are not usually directly dated. In this study, the formation ages of the Yellow River terraces in the Baode area in China were determined by dating [...] Read more.
Dating fluvial terraces has long been a challenge for geologists and geomorphologists, because terrace straths and treads are not usually directly dated. In this study, the formation ages of the Yellow River terraces in the Baode area in China were determined by dating fluvial deposits overlying bedrock straths using optically stimulated luminescence (OSL) dating techniques. Seven terraces (from the lowest terrace T1 to the highest terrace T7) in the study area were recognized, and they are characterized by thick fluvial terrace deposits overlaid by loess sediments. Twenty-five samples from nine terrace sections were dated to about 2–200 ka. The OSL ages (120–190 ka) of the fluvial samples from higher terraces (T3–T6) seem to be reliable based on their luminescence properties and stratigraphic consistency, but the geomorphologic and stratigraphic evidence show that these ages should be underestimated, because they are generally similar to those of the samples from the lower terrace (T2). The formation ages of the terrace straths and treads for the T1 terrace were deduced to be about 44 ka and 36 ka, respectively, based on the deposition rates of the fluvial terrace deposits, and the T2 terrace has the same strath and tread formation age of about 135 ka. The incision rate was calculated to be about 0.35 mm/ka for the past 135 ka, and the uplift rate pattern suggests that the Ordos Plateau behaves as a rigid block. Based on our previous investigations on the Yellow River terraces and the results in this study, we consider that the formation ages of terrace straths and treads calculated using deposition rates of terrace fluvial sediments can overcome problems associated with age underestimation or overestimation of strath or fill terraces based on the single age of one fluvial terrace sample. The implication is that, for accurate dating of terrace formation, terrace sections should be systematically sampled and dated. Full article
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Open AccessLetter
ESR and Radiocarbon Dating of Gut Strings from Early Plucked Instruments
Methods Protoc. 2020, 3(1), 13; https://doi.org/10.3390/mps3010013 - 28 Jan 2020
Cited by 1
Abstract
Early European plucked instruments have recently experienced a great revival, but a few aspects remain unknown (e.g., the gauge of gut strings). Here we report, for the first time, that the electron spin resonance (ESR) signal intensity of oxidized iron, Fe(III), from gut [...] Read more.
Early European plucked instruments have recently experienced a great revival, but a few aspects remain unknown (e.g., the gauge of gut strings). Here we report, for the first time, that the electron spin resonance (ESR) signal intensity of oxidized iron, Fe(III), from gut strings at g = 2 increases linearly with age within a few hundred years. The signal increase in the remaining old strings on early instruments can be used to judge if they are as old as or younger than the instrument. Obtaining the authenticity information of gut strings contributes to the revival of the old instruments and the music. Full article
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Open AccessProtocol
Single-Grain Quartz OSL Characteristics: Testing for Correlations within and between Sites in Asia, Europe and Africa
Methods Protoc. 2020, 3(1), 2; https://doi.org/10.3390/mps3010002 - 26 Dec 2019
Cited by 2
Abstract
We studied the characteristics of the optically stimulated luminescence (OSL) signal of single-grain quartz from three sites in China, Italy, and Libya, including the brightness, decay curve and dose response curve (DRC) shapes, recuperation, and reproducibility. We demonstrate the large variation in OSL [...] Read more.
We studied the characteristics of the optically stimulated luminescence (OSL) signal of single-grain quartz from three sites in China, Italy, and Libya, including the brightness, decay curve and dose response curve (DRC) shapes, recuperation, and reproducibility. We demonstrate the large variation in OSL behaviors for individual quartz grains of different samples from different regions, and show that recuperation, sensitivity change, and reproducibility are independent of the brightness and decay curve shape of the OSL signals. The single-grain DRCs can be divided into at least eight groups with different characteristic saturation doses (D0), and a standardized growth curve (SGC) can be established for each of the DRC groups. There is no distinctive difference in the shape of OSL decay curves among different DRC groups, but samples from different regions have a difference in the OSL sensitivities and decay shapes for different groups. Many of the quartz grains have low D0 values (30–50 Gy), and more than 99% of the grains have D0 values of <200 Gy. Our results raise caution against the dating of samples with equivalent dose values higher than 100 Gy, if there are many low-D0 and ‘saturated’ grains. Full article
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Open AccessProtocol
Transferring Grains from Single-Grain Luminescence Discs to SEM Specimen Stubs
Methods Protoc. 2019, 2(4), 87; https://doi.org/10.3390/mps2040087 - 21 Nov 2019
Cited by 1
Abstract
The grain transfer protocol presents a step-by-step guide on how to successfully transfer positioned grains from a single-grain luminescence disc to a scanning electron microscope (SEM) specimen stub and how to transport them between laboratories. Single-grain luminescence analysis allows the determination of luminescence [...] Read more.
The grain transfer protocol presents a step-by-step guide on how to successfully transfer positioned grains from a single-grain luminescence disc to a scanning electron microscope (SEM) specimen stub and how to transport them between laboratories. Single-grain luminescence analysis allows the determination of luminescence characteristics for individual sand-sized grains. By combining such luminescence data with other grain properties such as geochemical composition, shape, or structure also at single-grain level, it is possible to investigate factors controlling luminescence signals or study other material properties. The non-luminescence properties are typically measured in another instrument; thus, grains need to be transferred between machines and sample holders, and sometimes also between laboratories. It is then important that the position of each grain is known and stable so that the properties from the same grain are compared. By providing an easily observable orientation marker on the specimen stub, the hundred numbered grains from the single-grain disc can be transferred and later identified when analyzed in the SEM. Full article
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