Variability in quartz OSL signals caused by measurement uncertainties: Problems and solutions

We simulated the variability in measured quartz optically stimulated luminescence (OSL) signals and dose response curves (DRCs) caused by measurement uncertainties, including counting statistics and instrumental irreproducibility. We find that these measurement errors can give rise to large variations in the observed luminescence signal and contribute to among-aliquot or among-grain scatter in DRCs and equivalent dose (D_e) values. Different measurement systems (i.e., luminescence readers) may have different counting statistics properties and, hence, may exhibit differing extents of variation in the observed OSL signal, even for the same sample. Our simulation shows that the random measurement uncertainties may result in some grains or aliquots being ‘saturated’ (that is, the measured natural signal is consistent with, or lies above, the saturation level of the measured DRC) and that the rejection of these ‘saturated’ grains may result in a truncated D_e distribution, with D_e underestimation for samples with natural doses close to saturation (e.g., twice the characteristic saturation dose, D₀). We propose a new method to deal with this underestimation problem, in which standardised growth curves (SGCs) are established and the weighted-mean natural signal (L_n/T_n) from all measured grains is projected on to the corresponding SGCs to determine D_e. Our simulation results show that this method can produce reliable D_e estimates up to 5D₀, which is far beyond the conventional limit of ∼2D₀ using the standard SAR procedure.     

A comparative study of sand- and silt-sized quartz fractions for MAR-VSL dating using loess-palaeosol deposits in southern Germany

Multiple-aliquot regenerative-dose violet stimulated luminescence (MAR-VSL) dating studies of the Chinese loess-palaeosol sequence in Luochuan using sand- and silt-sized quartz have previously produced inconsistent results; the VSL ages were in agreement with their independent ages up to ∼900 ka for sand-sized quartz, whereas the silt-sized VSL ages underestimated the independent chronology beyond ∼100 ka. Here we therefore evaluate the VSL dose response pattern of sand- (63–100 μm) and silt-sized (4–11 μm) quartz grains from the loess-palaeosol sequence in southern Germany in high resolution but with a limited age range up to ∼160 ka. All the samples studied benefit from good age control provided by reliable quartz optically stimulated luminescence (OSL) ages and fading corrected feldspar post-infrared infrared stimulated luminescence at 225 °C (pIRIR₂₂₅) ages, which can be used for assessing the validity of the estimated VSL ages. The comparison of the MAR standardised dose response curve (DRC) using regeneration doses up to ∼1000 Gy for both grain size fractions demonstrates that they are almost similar in shape with comparable characteristic saturation doses. The comparison of the natural and laboratory generated DRCs of each grain size reveals that they broadly overlap in the low dose range for both fractions, while in the high dose range the deviation between natural and laboratory DRCs is higher for the silt-sized quartz fraction. It is also shown that the magnitude of the characteristic saturation dose is dependent upon the size of the maximum given dose, especially for the silt-sized quartz. The constructed laboratory standardised DRCs to very high doses (up to ∼6000 Gy) showed continuous signal growth at high doses, particularly in the case of silt-sized quartz grains, thereby confirming our previous observation. The sand-sized quartz has a much less pronounced linear growth component and can therefore be considered more suitable for dating samples with equivalent doses falling on the high dose region of the DRC.     

Bleachability of pIRIR signal from single-grain K-feldspar

The high-temperature (e.g., >200 °C) post-infrared infrared (pIRIR) stimulated luminescence of feldspar has been widely used for dating, because it usually suffers negligibly from anomalous fading. However, compared to the quartz optically stimulated luminescence (OSL) or low-temperature (e.g., 50 °C) IR stimulated luminescence (IRSL) from feldspars, the high-temperature pIRIR signals have been shown to bleach more slowly and usually have high residual does of a few Gys or more, which limits its application to date relatively young samples and may cause problems for correcting residual dose/signal. In this study, we investigated the bleachability of K-feldspar pIRIR signals for individual grains. A significant variation in the bleachability of the pIRIR signal was observed among different K-feldspar grains from the same sample. Experiments show that such a variability may result in different residual doses for different grains and, consequently, additional scatter in D_e values. We present a method for quickly testing the bleachability of individual grains. Our result suggests that selecting the easy-to-bleach grains for D_e determination provides an efficient way to date young samples using high-temperature pIRIR signals, which avoids the compromise of using low-temperature pIRIR signals that may suffer from anomalous fading.     

The build-up of the laboratory-generated dose-response curve and underestimation of equivalent dose for quartz OSL in the high dose region: A critical modelling study

The application of a regeneration procedure for optically stimulated luminescence (OSL) dating requires that the dose-response curve (DRC) of a natural sample is the same as that of a laboratory-generated one. However, the build-up of the laboratory-generated DRCs of quartz has been widely reported in the literature, i.e., the laboratory-generated DRCs are significantly higher than the natural counterparts in the high dose region (above 150 or 200 Gy). This results in severe underestimation of equivalent dose (D_e) for quartz OSL in the high dose region during the application of a single-aliquot regenerative-dose (SAR) protocol. However, the potential mechanism governing the build-up of the laboratory-generated DRC is still unclear. In this study, we performed a comprehensive investigation of the natural and laboratory-generated OSL signals and DRCs using a kinetic model for quartz. We compared the differences in charge concentrations between natural and laboratory-irradiated aliquots following irradiation and monitored the competition for holes and electrons during preheat and stimulation, for the natural, regenerative, and test dose cycles. In the course of the modelling, we could see the build-up of laboratory-generated DRCs, the underestimation of D_e, and a double exponential saturation characteristic of the DRCs. We demonstrated a discrepancy in competition for electrons in the deep electron trap and recombination centres during stimulation between the natural, regenerative, and test dose cycles. The simulation results are directly relevant to quartz OSL D_e determination using the SAR protocol and reveal the mechanisms responsible for the experimentally observed different behaviours between natural and laboratory-generated DRCs.     

OSL and IRSL dating of raised beach sand deposits along the southeastern coast of Norway

Raised beach sand deposits along the southeastern coast of Norway were dated by optical (OSL) and infrared stimulated luminescence (IRSL) and the quartz and K-feldspar luminescence characteristics were described. Due to the poor quartz luminescence characteristics, only a limited number of samples were suitable for OSL dating. More promising are the K-feldspar extracts, with typical K-feldspar luminescence characteristics and no sign of fading. For equivalent dose (D_e) determination, sand-size quartz and feldspar extracts were used, applying a single aliquot regenerative (SAR) protocol. Both, OSL and IRSL D_e estimates show a wide distribution, unexpected for beach deposits. The calculated OSL and IRSL age estimates were generally in good agreement and the correctness of the ages was confirmed by independent age control. Because only a limited number of the quartz samples were suitable for OSL dating, IRSL dating of the K-feldspar represents an alternative to OSL quartz dating.     

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.     

Effects of the size of the test dose on the SAR protocol for quartz optically stimulated luminescence dating of loess in the eastern Tibetan Plateau

Dating of quartz by optically stimulated luminescence (OSL) has been revolutionized with introduction of the test dose (TD) in development of a measurement sequence known as the single-aliquot regenerative-dose (SAR), whereby a valid sensitivity correction for the luminescence signal is provided in the measurement cycle. However, the size of the TD used in the SAR protocol remains controversial. Previous studies show that the TD has little effect on the equivalent dose (D_e) for young samples in luminescence dating in which the applicability of different deposits varies greatly in different regions. However, detailed studies are lacking on how TD size affects SAR–OSL results of samples with a relatively high D_e range. In this study, typical loess samples with high D_e values (∼60 Gy–∼250 Gy) from the eastern Tibetan Plateau were selected to investigate the effects of variation in TD size on the quartz SAR–OSL protocol. Dose recovery tests show that a known dose could be recovered successfully by applying different TDs. Test dose size has an effect on shapes of regenerated dose–response curves (DRCs) and has different influences on D_es and characteristic saturation doses for quartz samples with a high dose range. A TD size of 20%–30% D_e is a good compromise for Tibetan loess with D_e of ∼60–120 Gy in the quartz SAR protocol, and a TD size larger than 30% should be considered for samples with a larger D_e. The results of this study highlight the importance of TD size in the SAR–OSL protocol for quartz samples with a high dose range.     

Infrared stimulated luminescence and radiofluorescence dating of aeolian sediments from Hungary

Anomalous fading of the infrared stimulated luminescence (IRSL) signal from the polymineral fine-grain and K-feldspar fractions of aeolian sediments from Hungary has been studied. The samples in this study have previously been dated using the multiple aliquot additive dose (MAAD) protocol to measure the IRSL signal. The IRSL measurements using MAAD were conducted ～4 weeks after the irradiation, making it difficult to assess to what extent these age estimates were affected by anomalous fading. In this study, equivalent doses were obtained using the single aliquot regenerative dose (SAR) protocol. The fading rate for each sample was calculated using the different IRSL components and different parts of the decay curve. For each sample, the middle part of the decay curve always showed a lower fading rate than the initial part of the decay curve. The difference between the fading rates for different parts of the decay curve was greater for the K-feldspars than for the polymineral fine grains. Fading corrected ages were calculated by integrating both the initial and the middle part of the decay curve. These ages were compared with optically stimulated luminescence (OSL) ages from quartz, infrared radiofluorescence (IR-RF) ages obtained from K-feldspars and also with independent ages, provided by radiocarbon dating of shells and charcoal, and uranium-series dating of travertine.     

Luminescence investigation of loess and tephra from Halfway House section, Central Alaska

Infrared stimulated luminescence (IRSL) properties of the Old Crow tephra and bracketing loess from the Halfway House site in Central Alaska are investigated in order to test newly developed techniques, including SAR and recently proposed fading corrections. Loess samples investigated show a standard growth of luminescence with regenerative dose while the tephra sample is less sensitive by an order of magnitude and saturates at lower dose. The growth curves obtained using multiple-aliquots regeneration (MAR) saturate at a higher value than those with the single-aliquot regeneration (SAR) protocol. Fading rate determinations for these samples are shown to be imprecise and no noticeable difference was observed between loess and tephra materials. Anomalous fading corrections using an average g value of 5% are applied to the natural test dose signal intensity using the dose rate correction (DRC) method. IRSL ages obtained for loess are in agreement with the expected age while the tephra age is lower than expected, suggesting the measured fading rate is underestimated for this material.     

Optical dating of a Japanese marker tephra using plagioclase

The luminescence characteristics of volcanic plagioclase from an andesitic tephra (Hakone-Tokyo pumice, Hk-TP) from Japan were studied in order to assess if optical dating of plagioclase could be applied to Quaternary tephra. The tephra was shown to contain two kinds of plagioclase grains, labradorite which had a smooth surface and bytownite with a rough surface. The aliquots consisting of smaller grains contained more bytownite; these showed higher luminescence sensitivity and a higher fading rate compared to the larger-grained aliquots containing only labradorite. The fading rates of both OSL and IRSL signals were similar for each grain size. However, the OSL signal showed severe thermal transfer which made it difficult to use for dating. Using the IRSL signal from grains ranging from 150 to 212 μm, an age was obtained in agreement with the independent evidence, once a small fading correction had been applied.     

Luminescence chronology of the upper part of the Stari Slankamen loess sequence (Vojvodina,Serbia)

A thick Middle and Late Pleistocene loess-palaeosol sequence is exposed at the Stari Slankamen section in the Vojvodina region situated in the south-eastern part of the Pannonian basin, Serbia. The profile exposes an about 45 m thick series of loess intercalated by at least eight pedocomplexes. Ten samples were dated by luminescence methods using a modified single aliquot regenerative dose (SAR) protocol for polymineral fine grains and for quartz extracts from the upper part of the Stari Slankamen loess sequence. The infrared stimulated luminescence (IRSL) and post-IR optically stimulated luminescence (OSL) signals from all polymineral samples showed anomalous fading, suggesting that the post-IR OSL signal is still dominated by feldspar OSL. The ages ranging from 4.6 to 193 ka were obtained after fading correction. These ages indicate that the loess unit V-L1L1, the weakly developed soil complex V-L1S1 and the loess unit V-L1L2 were deposited during marine isotope stage (MIS) 2, 3, and 4, respectively, and also indicate that the loess unit V-L2 is of the penultimate glacial age.     

Toward a luminescence chronology for coastal dune and beach deposits on Calvert Island,British Columbia central coast,Canada

The Quaternary geology of the central coast of British Columbia contains a rich and complex record of glacial activity, post-glacial sea level and landscape change, and early human occupation spanning the last ∼10,000 years. At present, however, this region remains a largely understudied portion of coastal North America. This study describes the luminescence characteristics of quartz and K-feldspar from coastal dune and beach sands on Calvert Island and develops a suitable optical dating protocol that will allow for a more rigorous chronology for post-glacial landscape evolution and human occupation on British Columbia's central coast. Luminescence signals from Calvert Island quartz are dim, and appear to lack the so-called “fast” component that is most desirable for optical dating. K-feldspar signals are sufficiently bright for optical dating. We test and refine a single-aliquot regenerative-dose (SAR) protocol for K-feldspar specific to Calvert Island samples through a series of dose recovery and preheat plateau tests. Two approaches for correcting a sample age for anomalous fading are compared and a correction for phototransfer is introduced and applied. Measured fading rates vary from sample to sample implying that, in this region, it is not sufficient to rely on two or three representative fading rates as has sometimes been done elsewhere. Refined age estimates show consistency with independent radiocarbon dating control and help identify radiocarbon-dated organic-rich sediments that have been reworked.     

A modified multi-elevated-temperature post-IR IRSL protocol for dating Holocene sediments using K-feldspar

A modified multi-elevated-temperature post-IR infra-red stimulated luminescence (MET-pIRIR) protocol is proposed for dating young samples of Holocene age using K-feldspar. The protocol utilizes a five-step MET-pIRIR measurement with a moderate preheating of 200 °C for 60 s, and a narrow IR stimulation temperature increment of 30 °C (i.e., the five measurement temperatures are 50, 80, 110, 140 and 170 °C). Using this method, the residual doses of the MET-pIRIR signals are generally less than 1 Gy. Holocene aeolian samples from Northern China were tested using the 30°C-increment modified MET-pIRIR method. The results demonstrate that similar ages from 140 °C to 170 °C were obtained for our samples, which were consistent with the quartz optically stimulated luminescence (OSL) ages. Based on this observation, the measurement procedures are further simplified to a three-step pIRIR protocol. The first IR stimulation at elevated temperature (110 °C) is used to remove the fading affected signals. This is followed by two steps of IR stimulation at high temperatures (140 and 170 °C) for equivalent dose (De) measurement. Dating results consistent with the expected ages have been obtained at stimulation temperatures of 140 and 170 °C. It is suggested that the first IR stimulation can effectively remove the fading component. The three-step pIRIR method has minimized the experimental procedures, while keeping the age plateau test.     

MET-post-IR IRSL luminescence dating of cobbles buried in fluvial terraces in the Northern Chinese Tian Shan

Cobbles can be used as an alternative to the conventionally employed sand-sized mineral luminescence dating. In piedmont environments, cobbles are much more abundant than sand-sized material. The IRSL₅₀ signal has been widely used in previous studies due to its greater sensitivity to exposure events. However, it is well known that the low temperature IRSL signal is more prone to fade than elevated temperature post-IR IRSL signal. In this study, to test the reliability and applicability of cobble sub-surface elevated temperature IRSL luminescence dating, six light-color granite cobbles and two sand-sized samples from silty sand lens were collected from a high terrace of Manas River on the northern piedmont of Chinese Tian Shan. A modified multi-elevated-temperature post-infrared infrared stimulated luminescence (MET-post-IR IRSL) protocol was applied. The age-temperature (A-T) plateau of MET-post-IR IRSL measurement was combined with the conventional age-depth (A-D) plateau in luminescence-depth profile to evaluate the resetting and fading of MET-post-IR IRSL signals. Uncertainties of grain-sizes of K-feldspar within solidified slices were also explored by μ-XRF mapping of potassium content. The A-T plateau was identified between MET-post-IR IRSL₁₇₀ and MET-post-IR IRSL₂₂₅ signals of one cobble, which suggested completeness of bleaching before burial and negligible anomalous fading during burial. This cobble yielded MET-post-IR IRSL₂₂₅ ages of 15.8 ± 2.6 ka and 19.0 ± 3.2 ka for top and bottom side, respectively. These MET-post-IR IRSL₂₂₅ ages were consistent with independent coarse-grained quartz MAM OSL ages (15.7 ± 3.6 ka and 14.8 ± 2.6 ka) of two sand-sized samples. The MET-post-IR IRSL₂₂₅ age of 16.0 ± 1.2 ka for the bottom side of another cobble was also consistent with the independent age, even without the A-T plateau. It was inferred to be caused by anomalous fading of MET-post-IR IRSL signals other than that stimulated at 225 °C by refering to the A-D plateau observed. Our results show that MET-post-IR IRSL measurement can be employed to determine the burial ages of cobbles. The A-T plateau, complemented with the A-D plateau, could be used to assess the reliability of burial ages of cobble luminescence dating from the view of bleaching and fading.     

Testing for sufficient signal resetting during sediment transport using a polymineral multiple-signal luminescence approach

We present a multiple luminescence signal measurement procedure that simultaneously measures six different luminescence signals from a single polymineral aliquot (i.e. multiple-signal, short MS-SAR approach). The six signals show different bleaching rates in bleaching experiments, ranging from rapid bleaching for the quartz dominated blue stimulated luminescence signal (measured at 125 °C, BSL-125), to the slow-bleaching polymineral thermoluminescence signal. The bleaching rate of the infrared stimulated luminescence (IRSL) measured at room temperature (IR-25) and elevated temperature post-IR IRSL (pIRIR-90, pIRIR-155, pIRIR-225) signals decrease with increasing measurement temperature. Owing to these different bleaching rates, the MS-SAR approach allows inference of the degree of bleaching, and thereby information on the transport history of sediments. We test this approach by applying the MS-SAR to four coastal samples from a well-monitored sand-nourishment site at the Dutch coast. Our results show that the proposed MS-SAR approach can be utilised to construct bleaching plateaus which provide an independent and time-effective measure of the degree of poor bleaching in a sediment sample based on the measurement of only a few large aliquots. We propose that the MS-SAR protocol can be used to profile the age, luminescence properties and degree of bleaching of minimal prepared polymineral. This pre-profiling will allow the selection of suitable samples for full luminescence dating analysis in a target-orientated and time-effective manner.     

Luminescence dating of old (>70 ka) Chinese loess: A comparison of single-aliquot OSL and IRSL techniques

The applicability of two different approaches in the luminescence dating of old (>70 ka) Chinese loess is investigated. Both SAR-OSL ages obtained on 63–90 μm quartz grains and SAR-IRSL ages obtained on 4–11 μm polymineral grains, for samples collected from two sites in the Chinese Loess Plateau (Luochuan and Dongchuan) are presented. The characteristics of the luminescence signals stimulated by blue and infrared light are investigated in terms of dose response and dose recovery, and as a function of age. Additionally, anomalous fading measurements from the 410 nm IRSL emission in polymineral fine-grains are reported. An average value of g_2days amounting to 3% per decade was measured and seems to be independent of site location and age. For the samples from Luochuan, independent age control (pedostratigraphy and palaeomagnetism) is available. At both sites, the SAR-OSL ages are always lower than the SAR-IRSL ages after they have been corrected for anomalous fading. It seems that the quartz-based SAR-OSL ages are accurate for the younger ages, but that they underestimate the true age of deposition for loess that was deposited about 60–70 ka ago. The fading-corrected SAR-IRSL ages are in better agreement with the pedostratigraphic age control (75 and 130 ka) and allow dating beyond the quartz OSL range. Based on our results, we suggest that conventional SAR-OSL and SAR-IRSL protocols at these sites should be restricted to samples of ages not exceeding 40–50  and 100–120 ka, respectively.     

Construction of a ‘global standardised growth curve’ (gSGC) for infrared stimulated luminescence dating of K-feldspar

We investigated the infrared stimulated luminescence (IRSL) and post-infrared IRSL (pIRIR) signals emitted by K-feldspars from sedimentary samples from Asia, Europe and Africa using a single-aliquot multiple elevated temperature (MET) stimulation procedure. For separate aliquots of the same sample, we show that variation among the dose response curves (DRCs), or growth curves, constructed from the regenerative dose signal (L_x), the test dose signal (T_x, an indicator of luminescence sensitivity) and the sensitivity-corrected signal (L_x/T_x) can be largely eliminated by normalising the DRCs using one of the regenerative dose signals; we call this procedure ‘regenerative-dose normalisation’ or re-normalisation. Furthermore, for the MET-pIRIR signals measured at 250 °C, we find that different samples have re-normalised DRCs that follow the same growth function, despite the samples differing significantly in terms of their geological provenance, sedimentary context, equivalent dose (D_e) and luminescence sensitivity. This common feature offers the potential to establish a ‘global standardised growth curve’ (gSGC) for different samples of K-feldspar, and thereby enable D_e values to be estimated for a large number of single aliquots by projecting the re-normalised natural signals on to the gSGC. For the 18 samples investigated in this study, we find that D_e estimates obtained from the gSGC are consistent with those obtained using full single-aliquot regenerative dose (SAR) procedures for doses of up to ∼1600 Gy. The establishment of a gSGC would greatly reduce the time required to date older samples using K-feldspar, as regenerative doses of several hundreds to a few thousands of Gy are typically delivered to each aliquot in each SAR cycle.     

Testing the use of feldspars for optical dating of hurricane overwash deposits

The geological record preserved in coastal salt marshes provides an opportunity to determine past hurricane activity during the Late Holocene in New England, USA. High precision dating is important to correlate overwash sand layers associated with hurricane strikes between different sites along the coastline. Three different optical dating methods have been tested and compared with independent age control; i) optically stimulated luminescence from quartz, ii) infrared stimulated luminescence from K-feldspar, and iii) a subtraction method.Quartz and K-feldspar dating results for three samples in a core from Round Hill Beach Marsh are in stratigraphic order and they are consistent within errors with radiocarbon ages and with each other. Subtraction dating results agreed with the quartz and K-feldspar ages for two of the three samples, but the subtraction age of the youngest sample gave an age underestimate. Replicate equivalent dose values from quartz showed a larger variation than those from feldspars, and this resulted in larger errors for the quartz and subtraction ages than those based on feldspars. K-feldspar yields the most precise optical ages, but is complicated by the need to correct for anomalous fading. Both quartz and K-feldspar are suitable for optical dating of hurricane overwash deposits in New England.     

Luminescence dating of shoreline sediments indicates a late deglacial lake-level rise of Selin Co on the central Tibetan Plateau

The palaeo-shorelines around the lakes on the Tibetan Plateau can be used to reconstruct water level variations, which serve as sensitive indicators of hydroclimate change. Extensive studies have been carried out to constrain the Holocene lake level fluctuations by dating shorelines with a variety of methods (e.g., luminescence, ¹⁴C, ¹⁰Be and U–Th series). In comparison, the timing of the lake level variations during the last glacial and subsequent deglaciation periods has been rarely studied. The driving factors of such changes, therefore, remain elusive. In this study, we performed a detailed luminescence dating investigation on six samples taken from a nearshore sedimentary outcrop in the south of Selin Co basin. The post-IR IRSL signals measured at 225 °C (pIRIR₂₂₅) on sand-sized K-feldspar grains demonstrated a generally good behavior and yielded reliable chronologies, while the optically stimulated luminescence (OSL) signals of quartz showed systematical age underestimation, which was attributed to anomalous fading. Six pIRIR₂₂₅ ages ranging from 15 to 10 ka suggested that the lake level of Selin Co during the last deglaciation reached up to 40–45 m high above the modern lake level. In view of the regional precipitation and temperature proxy records, we consider that the glacier meltwater supply has likely been the primary contributor to the lake highstands during the last deglaciation.