Assessment of diagnostic tests for evaluating the reliability of SAR De values from polymineral and quartz fine grains

In this study, we applied optically stimulated luminescence (OSL) dating to two fine grain sediment samples collected at Jeongokri, Korea. A single aliquot regenerative dose (SAR) procedure was applied to both polymineral grains and to chemically isolated (H₂SiF₆) quartz grains of 4–11 μm diameter. For polymineral fine grains, the OSL IR depletion ratio and the equivalent dose (D_e) plateau test appear to be equally sensitive indicators of appropriate IR stimulation time for use in the ‘double SAR’ protocol. Additionally, the OSL IR depletion ratio test gives an indication of the relative mineral composition of the samples, hence providing an assessment of the likelihood of obtaining a quartz-dominated [post-IR] OSL signal. Use of higher preheat temperatures would assist in thermally eroding the non-quartz component of the [post-IR] OSL signal from polyminerals. For the quartz fine grains, data from both natural D_e determinations and laboratory dose recovery tests are required to identify the appropriate preheat temperatures for dating, due to problems of thermal transfer. This phenomenon is particularly exaggerated for these samples due to the large D_e values (≥350 Gy) and hence low slope of the dose–response curve. The double SAR method cannot be applied ubiquitously, even after careful and rigorous study of one sample from a section. Quartz OSL dating using a range of preheat temperatures is suggested to be the most suitable method for OSL dating of fine grain sediments.     

Luminescence dating of quartz using an improved single-aliquot regenerative-dose protocol

Single aliquot protocols are now widely used as a means of measuring the equivalent dose (D_e) in quartz and feldspar optical stimulated luminescence (OSL) dating of both heated and sedimentary materials. The most recent of these is the single-aliquot regenerative-dose (SAR) protocol, first suggested by Murray and Roberts (Radiation Measurements 29, 503–515, 1998). In this approach, each natural or regenerated dose OSL measurement is corrected for changes in sensitivity using the OSL response to a subsequent test dose (10–20% of D_e). If the sensitivity correction is adequate, then the corrected OSL response should be independent of prior dose and thermal/optical treatment, i.e. there should be no change in the sensitivity-corrected dose–response curve on remeasurement. Here we examine the interpretation of the sensitivity corrected growth curve as a function of dose, and the effect of changing measurement conditions (e.g. preheat temperature, size of test dose, stimulation temperature) on the estimation of D_e. The dependence of the dose response on prior treatment is tested explicitly, and the significance of thermal transfer discussed. It is concluded that a robust SAR protocol is now available for quartz, and that it is applicable to a wide range of heated and unheated materials.     

A comparison of natural- and laboratory-generated dose response curves for quartz optically stimulated luminescence signals from Chinese Loess

It has previously been observed that laboratory-generated quartz optically stimulated luminescence (OSL) signals from different samples have similar dose response curves (DRCs) after they are normalized using a test dose. It therefore seems likely that growth of the normalized signal due to natural irradiation of quartz may also follow a general dose response curve. The existence of such a curve is investigated by constructing a natural DRC from the test dose-normalized natural OSL signals of seven samples from the Luochuan section of the Chinese Loess Plateau. The same aliquots are then used to build single aliquot regenerative (SAR) DRCs, making it possible to compare the natural and laboratory constructed curves. Two main differences are observed. Firstly, the laboratory-generated DRCs are best fitted with double saturating exponential functions whereas the natural DRC is equally well fitted with a single saturating function. Secondly, in the laboratory-generated DRCs the normalized OSL signal continues to increase at high laboratory doses (>500 Gy), whereas no growth is seen at these doses in the equivalent natural DRC. These differences between natural- and laboratory-generated DRCs are still apparent even if data are manipulated to isolate the fast component, or if a sensitivity corrected multiple aliquot regenerative (SC-MAR) dose procedure is used. This suggests that the observed differences are not due to the influence of different components or inter-regenerative dose cycle sensitivity changes. The divergence between the natural- and laboratory-generated DRC means that the current maximum limit of quartz OSL dating at the Luochuan section is 150 Gy, as D_e estimates above this value are likely to be underestimations.     

Dose dependence of thermally transferred optically stimulated luminescence signals in quartz

The thermally transferred optically stimulated luminescence (TT-OSL) responses of chemically purified fine-grained quartz from seven loess-like samples from Korea are presented. In particular, the experimental procedures used to separate the dose-dependent (recuperated OSL, ReOSL) and dose-independent parts of the signal were explored. The OSL signals used to monitor the sensitivity changes that take place during the measurement sequences used to determine the equivalent dose were investigated. A single aliquot procedure was used for the TT-OSL measurements and resulted in linear growth of the ReOSL with dose up to at least 2 kGy. For this suite of samples, a standardised growth curve (SGC) was constructed for the ReOSL, tested with dose recovery experiments, and was used to obtain D_e values for the seven samples.     

On the intrinsic accuracy and precision of the standardised growth curve (SGC) and global-SGC (gSGC) methods for equivalent dose determination: A simulation study

In optically stimulated luminescence (OSL) dating, the single aliquot regenerative-dose (SAR) method has been used extensively for determining equivalent doses (D_e) in quartz. A variation of the SAR method is the “standardised growth curve” (SGC) method, which has been used as an efficient procedure to save measurement time during dating studies. During the application of the SGC method one establishes the SGC and calculation of the D_e of an aliquot requires only measurement of the standardised natural dose signal. Recently, a “global standardised growth curve” (gSGC) method was developed as an improved version of the SGC procedure. During the application of the gSGC method, the growth curves are re-normalised using sensitivity-corrected signal corresponding to one of the regenerative doses. Subsequently the D_e of an aliquot is estimated using the sensitivity-corrected natural dose signal and an additional sensitivity-corrected regenerative dose signal as well as the established gSGC. In the present study, simulations are performed to assess the intrinsic accuracy and precision of the SGC and gSGC D_e estimates. The results of our simulations validate that the gSGC method is intrinsically more precise than the SGC method and is also more accurate for doses greater than 210 Gy. Several factors which affect the reliability of the two methods are investigated.     

The estimation of basic experimental parameters in the fine-grained quartz multiple-aliquot regenerative-dose OSL dating of Chinese loess

The sensitivity-corrected multiple-aliquot regenerative-dose (MAR) protocol provides a reliable approach for fine-grained quartz optically stimulated luminescence (OSL) dating. For reliable estimation of the equivalent dose (D_e), we investigated certain basic experimental parameters in the fine-grained quartz MAR OSL dating of Chinese loess. (1) For suitable bleaching of the natural OSL signal of the regenerative-dose aliquots, the effect of bleaching duration using sunlight, SOL2 and blue LEDs on D_e was studied, and it is found that the appropriate method is a short-duration SOL2 (e.g. 5 min) or blue LEDs (e.g. 60 s) bleaching. (2) To select the appropriate test dose, the relationship between the test dose and D_e was investigated based on three samples having D_e values of approximately 11, 31 and 137 Gy respectively. It is suggested that the test dose for sensitivity correction may be limited to less than approximately 10–20 Gy. (3) Three commonly used fitting modes for quartz OSL growth curve were compared at three regenerative-dose scales. The results indicate that the mode of two saturating exponential functions plus a constant is appropriate and universal. (4) The comparison of D_e values derived using OSL approach with those obtained using the recuperated OSL (ReOSL) protocol shows that the reliable D_e estimation in the fine-grained quartz MAR OSL dating of Chinese loess may be limited to less than approximately 300 Gy. (5) The comparison of growth curves for 18 samples from the Weinan, Xifeng and Jingyuan sites shows that it is feasible to construct a standardized growth curve (SGC) for fine-grained quartz OSL signal in the Chinese Loess Plateau (CLP).     

The a-value of polymineral fine grain samples measured with the post-IR IRSL protocol

Recent post-IR IRSL (pIRIR) dating studies using polymineral fine grains assumed that the a-values obtained for the IRSL signal at 50 °C and the pIRIR signal at higher temperatures (e.g. 225 °C) are identical. However, the a-value of a sample depends on the stimulation method, and the assumption mentioned above remains to be tested. Using five polymineral fine grain samples, this study investigates whether a common a-value can be used for both the IR and the pIRIR signals. Applying the pIRIR protocol, the a-values were measured with three different methods of signal resetting (optical bleaching, end of SAR cycle, heating). In addition, uncorrected α- and β-irradiation induced growth curves were determined for three samples and fitted with single saturating exponential functions. For the investigated samples we found significant mean differences, 0.023 ± 0.012 and higher, in the a-values determined for the IR₅₀ and pIRIR₂₂₅ signals. Synthetic a-values deduced from uncorrected multiple-aliquot dose response curves seem to confirm this observation. Although, in summary, our results indicate that the practice of using a common a-value should be carefully re-considered, the physical reasons remain to be determined.     

Empirical insights into multi-grain averaging effects from ‘pseudo’ single-grain OSL measurements

In this study we assess the signatures of multi-grain averaging effects for a series of sedimentary samples taken from the archaeological site of Hotel California, Atapuerca, Spain. We focus on the special case of equivalent dose (D_e) measurements made on single-grain discs that contain more than one quartz grain in each of the individual grain-hole positions with the aims of (i) providing insight into the nature and extent of averaging effects in very small multi-grain aliquots of sedimentary quartz, and (ii) assessing the suitability of ‘pseudo’ single-grain D_e measurements for this particular dating application. Pseudo single-grain OSL measurements made on standard discs loaded with 90–100 μm grains (equivalent to ～30 grains per hole) yield significantly different D_e distribution characteristics and finite mixture model (FMM) burial dose estimates compared with single-grain OSL measurements. Grains with aberrant luminescence behaviours, which are routinely rejected during single-grain analysis, exert strong averaging effects on the pseudo single-grain and multi-grain aliquot D_e distributions. Grain-hole averaging effects arising from pseudo single-grain measurements also give rise to ‘phantom’ dose components and are apt to provide bias assessments of quartz signal characteristics and grain type classifications. Though this is a site-specific study, it serves as a cautionary note for interpretations of other pseudo single-grain OSL and D_e datasets – particularly those obtained from measurements of discs containing several tens of grains per hole and those derived from complex depositional environments. The use of custom single-grain discs drilled with smaller sized grain holes is recommended as a means of limiting grain-hole averaging effects when dealing with very fine (<180 μm) sediments.     

Quartz from southern Africa: sensitivity changes as a result of thermal pretreatment

Sensitivity changes are known to occur in quartz during luminescence measurement procedures. Accurate single-aliquot equivalent dose (D_e) evaluations can be made only if the experimental procedure applied causes no sensitivity change, or can correct for it. The quartz single-aliquot regenerative-dose (SAR) protocol developed by Murray and Wintle (Murray, A.S., Wintle, A.G., 2000. Luminescence dating of quartz using an improved single-aliquot regenerative-close protocol. Radiation Measurements 32, 57–73) incorporates a sensitivity correction procedure that was developed using measurements made on a single sample from Australia. This paper presents experimental data designed to test the applicability of this correction procedure to quartz extracted from two southern African sediments. The results indicate that accurate corrections are made using this protocol irrespective of the direction and magnitude of the sensitivity change. The implications for routine D_e evaluation are discussed.     

Spatially-resolved thermoluminescence from snail opercula using an EMCCD

In recent years opercula of the snail species Bithynia tentaculata have been shown to emit thermoluminescence (TL) signals that can be used to determine equivalent dose, and may be capable of dating events throughout the entire Quaternary period. Concentric growth lines are a notable feature of almost all B. tentaculata opercula, but it is not known whether the luminescence emitted by the opercula is influenced by these structures. This study uses a newly developed EMCCD imaging system to measure the TL signals from opercula. A combination of microscopic analysis of the opercula using visible imagery, and measurement of the TL using the EMCCD system has been undertaken. Variations in TL intensity and equivalent dose (D_e) are seen, but the two are not correlated. Changes in TL intensity broadly mimic the concentric growth structures, but the largest variations in intensity are between different margins of the opercula, not individual growth bands. The EMCCD system makes it possible to produce a two dimensional map of the D_e measured from an operculum. Dose recovery experiments give D_e values that are consistent with each other across the whole opercula. Measurement of the D_e arising from irradiation in nature shows significant variability across a single operculum, but at present the reason for this variability is unknown.     

Luminescence sensitivity changes of polymineral fine grains during IRSL and [post-IR] OSL measurements

Sensitivity changes during measurement sequences of infra-red-stimulated luminescence (IRSL) and post-IR optically stimulated luminescence (OSL) are presented for a sample of loess from northwestern China. Together with a dose recovery experiment, the results are used to investigate the ratio of 2.4 found for the D_e values (for IRSL and [post-IR] OSL) obtained when using a single-aliquot regenerative-dose (SAR) protocol in which both D_e values are obtained in a single sequence of measurements. Responses to test doses for both the IRSL and [post-IR] OSL show progressive luminescence sensitivity changes with repeated measurement cycles, with a slight dose dependence for the IRSL. In addition, five modified SAR procedures were used, varying preheats, filter combinations and method of measuring the luminescence signal. The D_e values for all IRSL measurements were at least 50% greater than those for the [post-IR] OSL signal. A modified SAR sequence was also applied in which 0.1 s stimulations (using both IR and blue light sources) were made between all sample treatments. A lack of consistency in the measured luminescence sensitivity of the natural IRSL signal suggests that the [post-IR] OSL signal provides the more reliable value of D_e.     

Using optically stimulated electrons from quartz for the estimation of natural doses

A flow-through Geiger-Müller pancake electron detector attachment has been fitted to a standard Risø TL/OSL reader enabling optically stimulated electrons (OSE) to be measured simultaneously with optically stimulated luminescence (OSL). Using this detector, OSE and OSL measurements from natural quartz samples are studied to examine the possible use of OSE as a chronometer. First the relative variability in OSE and OSL growth curve shapes and the effect of preheat on these are presented, and from these curves, conclusions are drawn concerning the charge movement in natural quartz. Secondly, a dose recovery test shows that OSE can successfully recover a laboratory dose of 300 Gy given before any laboratory thermal treatment, for preheating temperatures between 160 and 260 °C. Furthermore, for the first time natural OSE decay curves are detected and these signals are used to estimate a burial dose using the single-aliquot regenerative-dose (SAR) procedure. Finally, a comparative study of the equivalent doses estimated using both OSE and OSL from 10 quartz samples are presented, and it is shown that OSE has a significant potential in retrospective dosimetry.     

Yellow stimulated luminescence from potassium feldspar: Observations on its suitability for dating

Yellow stimulated luminescence (Y-OSL) is the light detected from potassium-rich feldspars at 410 nm under stimulation by a yellow light source emitting 590 nm. The investigation of this study aimed at understanding basic luminescence physics of Y-OSL in order to assess the suitability of the technique for dating. The Y-OSL signal properties tested were signal intensity, thermal assistance, thermal stability, sensitivity to daylight and the suitability of a single aliquot regenerative (SAR) protocol to be employed for equivalent dose (D_e) estimation. D_e measurements were conducted on samples of Holocene, last glacial and Tertiary age. The tests were undertaken on sedimentary feldspar separates extracted from aeolian, fluvial and coastal deposits.Results from experiments show that the signal intensity increases by measuring Y-OSL at elevated temperature suggesting thermal assistance characteristics similar to infrared stimulated luminescence (IRSL). The yellow stimulated signal remains unaffected by preheat temperatures up to ～200 °C suggesting higher thermal stability than the IRSL signal. The Y-OSL signal is less light sensitive than the IRSL signal and D_e residuals obtained from modern samples are up to 7 Gy indicating suitability of the technique for ‘older’ and well-bleached sediments. The dose recovery tests successfully recovered the given dose if the specific light sensitivity of Y-OSL is taken into account. For every sample Y-OSL D_e values obtained by a single aliquot regenerative dose protocol (SAR) are higher than those obtained by an IRSL SAR approach. From these results we infer high thermal stability and a minimal anomalous fading of the Y-OSL signal. We conclude that Y-OSL has a high potential to date Quaternary sediments that were sufficiently bleached in nature.     

The potential of luminescence signals from electronic components for accident dosimetry

This study investigated the optically stimulated luminescence of a large number of electronic components extracted from both old and new generation mobile phones and chip modules of phone cards. Most resistors and all chip modules studied present a linear dose response (R > 0.99) in the dose range investigated (200 mGy up to 6 Gy, respectively 10 Gy), while capacitors, inductors and integrated circuits generally have a non-linear growth (exponential or cubic). For our experimental setup, an average specific luminescence of ∼20,000 cts in 2 s/Gy (n = 10) and ∼6000 cts in 2 s/Gy (n = 14) was obtained for two types of chip modules with a relatively high degree of homogeneity (relative standard deviation of 23% and 31%) and a minimum detectable dose of 7 mGy for immediate measurement. The investigated signals show small sensitivity changes (generally <10%) after repeated cycles of irradiation and readout. Preliminary fading measurements are presented. It can be concluded that most mobile phones and phone card components have a significant potential as retrospective luminescence dosimeters.     

Test and optimization of two routine dosemeters for the dose quantity Hp(3)

The individual monitoring service Seibersdorf uses two different passive dosemeter types based on thermo luminescence (TL) detectors for monitoring occupationally exposed persons in Austria. Whole body personal dosemeters for the personal dose equivalent quantities H_p(10) and H_p(0.07) worn on the trunk and dosemeters for the extremities for H_p(0.07) worn on a finger or wrist. Both routine dosemeters were calibrated and tested in terms of the personal dose equivalent H_p(3) assuming that the whole body dosemeter is worn on the chest (without or above a lead apron) and the modified ring/wrist dosemeter using a special strap worn on the forehead near the eyes (head band dosemeter). The test results show that it is possible to measure the dose quantity H_p(3) with these dosemeters that were originally not designed for this dose quantity. Only changes in the dose calculation algorithm and in the choice of the reference radiation quality were necessary to fulfil the requirements given in international standards for passive dosemeters in a wide energy (20 keV–1.3 MeV) and angular range (0°–60°).     

Variations in luminescence properties of single quartz grains and their consequences for equivalent dose estimation

In this paper examples of variability of luminescence properties between single grains of quartz extracted from natural samples or from crushed single crystals are shown. It is demonstrated how measurements of glow curves, PSL (photon stimulated luminescence) decay curves, thermal activation characteristics using multi-grain aliquots can lead to a misinterpretation of the obtained data. The possible consequences for different D_E estimation techniques applied to multi-grain aliquots or to single grains and normalisation techniques applied to multi-grain aliquots are discussed. In particular pre-dose, multi-aliquot additive, and single grain PSL SAR D_E estimation methods are considered.     

Improving the accuracy and precision of equivalent doses determined using the optically stimulated luminescence signal from single grains of quartz

Optically stimulated luminescence (OSL) measurements of quartz are widely used to measure equivalent dose (D_e). At radiation doses above ～100 Gy, saturation of traps results in a decrease in the rate of growth of the OSL signal, and this makes calculation of D_e increasingly difficult. A series of dose recovery experiments was undertaken using single grains of quartz from Kalambo Falls, Zambia to explore saturation of single grains. When the OSL signal from many grains is averaged, the characteristic dose (D₀) is 47 Gy, typical of published values for quartz. However, D₀ for individual grains varies from ～10 to 100 Gy. Doses up to two times the average D₀ could be accurately recovered, but above this dose the D_e became increasingly underestimated. Overdispersion for this type of experiment should be zero, but was observed in all data sets; furthermore the value of overdispersion increased with D_e. An additional acceptance criterion, the Fast Ratio, is suggested for single grain OSL analysis. This criterion assesses the relative contribution of the fast component of the OSL signal. Including this as an additional acceptance criterion leads to an improved precision, with overdispersion reduced to zero, and improved accuracy in dose recovery at high doses.     

Paper I: The use of measurement-time dependent single-aliquot equivalent-dose estimates from quartz in the identification of incomplete signal resetting

The identification of incomplete signal re-setting of optically stimulated luminescence signals in sedimentary quartz is a vitally important step in the continued improvement of optical dating. It is shown that narrow spectrum (blue-green) laboratory partial bleaching of aliquots of natural sedimentary quartz has a significant effect on equivalent dose (measured using a single aliquot procedure) calculated as a function of measurement time (D_e(t)). The blue-green stimulation spectrum mimics that found underwater and the results suggest that incomplete re-setting of waterlain sediments may be possible using the D_e(t) method.     

Minimal-disturbance measurement as a specification in von Neumann's quantal theory of measurement

In von Neumann's theory an incomplete observableA is measured by measuring any complete observableB whose functionA is. This procedure is narrowed down in this paper by the additional requirement of preservation of the sharp value of any observable compatible withA. The requirement is shown to be equivalent to the unique change of state:ρ → (trρP _n)^?1 P _nρP_n (P _n is the eigenprojector ofA corresponding to the obtained eigenvaluea _n, ρ is the statistical operator of the initial state, and by assumption trρP _n > 0). This characterises the minimal-disturbance measurement. A necessary and sufficient condition is derived for the selection of the above observableB so that its measurement implies the minimal-disturbance measurement ofA. For arbitraryρ andA, there exists aB satisfying the condition. Hence, this constitutes a reasonable specification within von Neumann's theory, reducing the latter to the physically preferable minimal-disturbance measurement theory.