Investigating the contribution of recuperated TL to post-IR IRSL signals in a perthitic feldspar

Using a museum specimen of perthitic feldspar, the characteristics of post-IR IRSL production at 200 °C after different prior IR bleaching at 100 °C were investigated. It was found that the post-IR IRSL signal had an isothermal TL contribution that was unexpected following a previous preheat at 320 °C; this is the result of isothermal decay of recuperated TL peaks resulting from photo-transfer that occurred when the previous IRSL signal was measured at a lower temperature. The isothermal TL contribution to the post-IR IRSL signal depends on prior IR bleaching conditions. Since the recuperated TL signal comes from photo-transfer during IRSL production, this signal should also suffer from anomalous fading. Thus, it is suggested that this isothermal TL contribution to the measured post-IR IRSL is removed by the inclusion of an additional step, a cut-heat to 300 °C, in the post-IR IRSL dating protocol.     

Natural variations in the properties of TL and IRSL emissions from metamorphic and volcanic K-feldspars from East Africa: Assessing their reliability for dating

The elevated temperature infrared stimulated luminescence (IRSL) and post-IR IRSL signals of potassium (K)-feldspars have recently garnered attention for their minimal rates of anomalous fading. The post-IR IRSL signal has been used to obtain age estimates for geological deposits, mostly in Europe. Studies on the behaviour of the IRSL and post-IR IRSL signals of K-feldspars from a wider range of geographic regions and depositional contexts are needed, particularly for regions where the OSL signal from quartz is poorly behaved. Discrepancies in the literature regarding the behaviours of the IRSL and TL signals of K-feldspars also highlight the need to characterise the behaviours of samples from a wide variety of contexts. This paper begins to address this problem by characterising and comparing the IRSL signals of a metamorphic and a volcanic K-feldspar sample from two sites in East Africa, a region in which the OSL signal from quartz has generally proven problematic for dating. We demonstrate that the metamorphic and volcanic K-feldspars have substantially different TL glow curves that respond differently to IR stimulation. The sample of metamorphic K-feldspar from Tanzania (MR9) has a peak at 430 °C that is associated with the IRSL signal and an optically less-sensitive peak at 350 °C, while the sample of volcanic K-feldspar from Ethiopia (MB3) exhibits a single broad TL region centred at ～230 °C that responds differently to IR stimulation. Differences in the change of IRSL decay curve shape with stimulation temperature suggest that the processes of IRSL production many vary between the two samples. Using dose recovery tests, we demonstrate that the IRSL (50 °C), IRSL (225 °C) and post-IR IRSL (50 °C, 225 °C) signals of sample MR9 are suitable for dose and age estimation using the single-aliquot regenerative-dose procedure, while those of sample MB3 are less suitable. The post-IR IRSL signal of the latter sample performs poorly in tests of SAR suitability and the three signals exhibit extremely high fading rates over laboratory timescales (g_2days > 19%/decade).     

Comparison of the properties of various optically stimulated luminescence signals from potassium feldspar

Various optically stimulated luminescence signals from K-feldspar have been used to determine the equivalent doses of sediment samples. Understanding the properties of these optical signals is critical to evaluate their applicability and limitations to optical dating. In this paper, some properties of IRSL, post-IR OSL and post-IR IRSL signals (detected in the UV region using U-340 filters) from a museum sample of K-feldspar were investigated by analyzing the relationships between optical and TL signals, and the effect of optical bleaching and heating on optical signals. The trap parameters of the different optical signals were calculated using the pulse annealing method. The results show that this sample exhibits two regenerated TL peaks at ～140 and ～330 °C. Corresponding to the low temperature TL peak, the OSL and post-IR OSL signals appear to be more associated with lower temperature TL than the IRSL signal measured at 50 °C. Corresponding to the high temperature TL peak, the post-IR IRSL signals mainly originate from the more thermally stable traps associated with the high temperature TL, compared with the IRSL and post-IR OSL signals. However, the post-IR IRSL_225 °C signal is shown to be hard to be bleached by blue light and simulated sunlight, compared with the IRSL_50 °C and low temperature post-IR IRSL signals. The implication for optical dating is that the elevated temperature post-IR IRSL signals can be preferentially applied over other signals from K-feldspar, but it is desirable that the effectiveness of the pre-depositional zeroing of these signals is assessed.     

A comparative study of the luminescence characteristics of polymineral fine grains and coarse-grained K- and Na-rich feldspars

The IRSL and post-IR IRSL (pIRIR) signal characteristics of polymineral fine grains are investigated and compared with those of K- and Na-rich feldspar extracts. TL signal loss after IR and pIRIR stimulations occurs mainly at around 320 °C for polymineral and Na-feldspar samples and around 410 °C for K-feldspar samples, when a preheat temperature of 250 °C for 60 s is used. After preheating to a higher temperature (320 °C for 60 s) all samples show a TL reduction around 410 °C in the blue detection window. Pulse annealing experiments for IRSL and pIRIR signals for preheats between 320 °C and 500 °C indicate that the signal stabilities are similar among the different feldspar types, when a higher preheat temperature (>320 °C) is used. Thermal activation energies for IRSL and pIRIR signals are largest in K-feldspar and smallest in polymineral fine grains, in both blue and UV detection windows for both fast time-resolved (TR) and continuous wave (CW) signals. These results suggest that IRSL and pIRIR signals in polymineral fine grains originate mainly from Na-feldspar grains; these signals are less thermally stable than those from K-feldspar, but a more stable signal (presumably from K-feldspar grains) can be obtained using a higher preheat temperature.     

Optically stimulated phosphorescence in orthoclase feldspar over the millisecond to second time scale

In the past, time-resolved IR stimulated luminescence (TR-IRSL) curves from feldspar have mainly been measured over a few hundred μs with the purpose of estimating the lifetimes of the components. In this study, we present the decay form of time-resolved IRSL and IR stimulated phosphorescence (IRSP) from orthoclase feldspar covering over 8 orders of magnitude (50 ns to ～7 s). A detailed characterisation of the slowly decaying signals (ms to s time scales) from feldspar is undertaken to obtain further insight into the role of re-trapping in both the IR stimulated luminescence (IRSL) and the relatively more stable post-IR IRSL signals. The decay form of the different signals examined here shows a weak dependence on preheat temperature and a strong dependence on stimulation temperature. Interestingly, the IRSP curves show a conspicuous kink of which the position is linearly dependent on the on-time duration.The data on thermal dependence of these signals might suggest that the decay behaviour of the time-resolved IRSL and phosphorescence signals mainly reflect the occupancy of electrons in the band tail states with a significant contribution from the shallow traps. This interpretation is supported by thermoluminescence (TL) curves showing the photo-transfer effect during short IR and post-IR IR stimulations.     

Testing Post-IR IRSL protocols for minimising fading in feldspars,using Alaskan loess with independent chronological control

Concern over anomalous fading has been the biggest single factor responsible for deterring the widespread use of the infra-red stimulated luminescence (IRSL) or thermoluminescence (TL) signal from feldspars for luminescence dating. There has therefore been great interest in the use of the recently proposed Post-IR IRSL signal, because it has been shown to significantly reduce the degree of anomalous fading observed in feldspars and therefore potentially provides a means of circumventing the issue. This study undertakes a systematic investigation into various preheat and Post-IR IRSL measurement conditions proposed in the literature, by using two samples from the Halfway House loess section in Alaska which bracket the Old Crow tephra which has been dated using fission track methods. Preheat plateau tests show a dramatic change in equivalent dose with Post-IR IRSL measurement conditions, and further tests reveal that these changes are driven by preheat temperature rather than Post-IR IR stimulation temperature. Dose recovery tests on laboratory-bleached material mimic the findings of the natural preheat plateau test data, and sensitivity change between the first and second Single Aliquot Regenerative dose (SAR) measurement cycle is found to be responsible. Comparison of the Post-IR IRSL ages with the independent age control shows that, for the samples in this study, the Post-IR IR signal stimulated at 290 °C is inappropriate for dating. However, use of lower preheat (250–300 °C) and Post-IR IR stimulation temperatures from 225 to 270 °C gave rise to ages which were in agreement with the independent age control.     

Basic thermoluminescent and dosimetric properties of Al2O3:C irradiated by pulse intensive electron beam

The effect of deep traps filled by a pulse electron beam on the thermoluminescent (TL) properties in Al₂O₃:C dosimetric crystals is studied. When the deep traps are filled, the dosimetric peak at 170 °C acquires a double-peak structure not present in the initial samples. The effect of the population of the deep centers having various nature (electron or hole traps) and energy depth on the shape of the dosimetric TL peak structure is analyzed. An assumption is made that in the temperature ranges of 350–500 °C and 650–750 °C, electron traps are emptied, whereas at T = 500–650 °C hole traps are emptied. The possibility of using the TL associated with deep traps in high-dose dosimetry of pulse electron beams is shown.     

Study of the relationship between infrared stimulated luminescence and blue light stimulated luminescence for potassium-feldspar from sediments

In luminescence measurements of potassium-feldspar (K-feldspar), both infrared (IR) and blue light (BL) can be used as stimulation sources. Component analysis suggests that the blue light stimulated luminescence (BLSL) measured at 60 °C from K-feldspar can be fitted using three components, namely fast, medium and slow. In order to explore the relationship between the origin of the infrared stimulated luminescence (IRSL) signal and the different components of the BLSL, five sets of experiments were conducted, namely post-IR BLSL (pIR-BLSL), post-BL IRSL (pBL-IRSL), pulse annealing tests, dose response and laboratory fading rate tests. It is observed that most of the IRSL signal can be bleached by BL, while the BLSL signal can only be partially bleached by the IR. The sources for IRSL are mainly associated with the fast and medium components of the BLSL signal.     

Optical depth of traps in AL2O3:C determined by the variable energy of stimulation OSL (VES-OSL) method

Standard methods of OSL measurements (CW-OSL or LM-OSL) do not allow for the direct determination of optical depth of traps. The variable energy of stimulation optically stimulated luminescence (VES-OSL) method gives such possibility. It consists in optical stimulation with the continuous increase of stimulation light energy and is analogous to the glow curve method in TL measurements. The VES-OSL curve shape and maximum position can be regulated by the stimulation photon flux, the rate of stimulation energy increase and by measurement temperature. This allows for detecting the OSL from very deep traps that give the TL signal overlapping with strong incandescence. The VES-OSL measurements carried out for Al₂O₃:C showed that traps having the optical depth between 2.0 and 2.8 eV are responsible for the OSL signal related to TL peak at about 200 °C. The OSL signal from the much deeper traps from the range 2.8–3.3 eV was also detected. The TL signal related do these traps cannot be detected below 500 °C.     

The relationship between thermal activation energy,infrared stimulated luminescence and anomalous fading of K-feldspars

A strong dependence of thermal activation energy (TAE) on infrared (IR) stimulation time for the infrared stimulated luminescence (IRSL) signal was observed for K-feldspar grains extracted from several sediments and granites from China. A TAE value as low as ～0.1 eV was observed at the beginning of IR stimulation and increased to ～0.45 eV after 90 s. For a trap depth of ～2 eV below the conduction band for the IRSL traps, the TAE value of ～0.45 eV is consistent with the energy gap between the excited states (～0.5 eV below the conduction band) and conduction band. This phenomenon is explained as the result of the coexistence of thermally assisted recombination via conduction band or band-tail states hopping and athermal tunnelling recombination of electrons from the excited states under IR stimulation, leading to the observation of a higher anomalous fading rate in the initial part of the IRSL decay curve.     

Assessing the impact of IR stimulation at increasing temperatures to the OSL signal of contaminated quartz

The purpose of the present study is to identify the effect of the increasing temperature IR stimulation to the component-resolved OSL luminescence signal of mixed quartz-feldspars material. Post IR OSL signals measured at 110 °C were analysed via only general order kinetic terms, while IR signals obtained at increasing temperatures were de-convolved using the sum of general order kinetics plus a tunnelling component. By increasing stimulation temperature, it was demonstrated that IRSL at temperatures above 50 °C does not only stimulate feldspar but also stimulates both fast and medium quartz OSL components. In the temperature range between 175 and 250 °C, the IRSL initial intensity is dominated by the fast OSL component. Estimated equivalent doses using either Post-IR₁₇₅.OSL₁₁₀ as well as IRSL₁₇₅ (with the indices indicating the measurement temperature) are in good agreement between each other, due to both stimulating quartz. Finally, the physical meaningfulness of the fitting parameters for the tunnelling component is also discussed.     

Luminescence from NaCl for application to retrospective dosimetry

The alkali halide NaCl (Common salt) is an environmentally-abundant phosphor of considerable potential for retrospective dosimetry and radiological event analysis due to its high sensitivity to ionising radiation when analysed by Thermoluminescence (TL), Optically-stimulated luminescence (OSL) or Infrared-stimulated luminescence (IRSL). We report here aspects of luminescence from NaCl relevant to the development of valid protocols for measurement of recent ionising radiation exposure. The timescale of interest in this application is from days to decades, hence our emphasis is on detection and characterisation of TL emission in the 100–300 °C range, and of OSL and IRSL emissions measured following only low temperature preheating (160 °C). A collection of 19 salt samples was assembled, including samples of rock salt and domestic salt produced by evaporation from brine. Analysis of TL emission spectral changes, together with previously reported TL, OSL and IRSL sensitivity changes, confirmed activation of sensitivity change by exposure to temperatures exceeding 160 °C. Kinetic analysis using Chen's method found E = 0.943 eV and s = 5.1 × 10¹¹ s^?1 for the 100 °C TL peak, giving a lifetime at 20 °C consistent with previous calculations and in the range of 7–14 h.     

Investigations of the post-IR IRSL protocol applied to single K-feldspar grains from fluvial sediment samples

The post-IR IRSL protocol with single K-feldspar grains was applied to three samples taken from a fluvial sedimentary sequence at the archaeological site of the Dali Man, Shaanxi Province, China. K-feldspar coarse grains were extracted for measurement. Approximately 30–40% of the grains were sufficiently bright to measure, and after application of rejection criteria based on signal strength, recuperation, recycling ratio and saturation dose, ～10–15% of the grains were used for D_e calculation. The relationship of signal decay rate and form of D_e(t) with the recovery dose were investigated. The dose recovery ratios of the samples after initial bleaching with the four different light sources were within uncertainties of unity. No anomalous fading was observed. The over-dispersion of the recovered dose and D_e values were similar, suggesting neither incomplete resetting of the post-IR IRSL signals nor spatially heterogeneous dose rates significantly affected the natural dose estimates. The values of D_e obtained with the single K-feldspar grain post-IR IRSL protocol were in the range ～400–490 Gy. Combining all of the measured single-grain signals for each of the individual samples (into a ‘synthetic single aliquot’) increased the D_e estimates to the range ～700–900 Gy, suggesting that the grains screened-out by the rejection criteria may have the potential to cause palaeodose over-estimation, although this finding requires a more extensive investigation. Thermally transferred signals were found in the single K-feldspar grains post-IR IRSL protocol, and the proportion of thermally transferred signal to test-dose OSL signal (stimulation at 290 °C) from the natural dose was higher than from regenerative doses, and the proportion was grain- and dose-dependent. As such, TT-post-IR IRSL signals at 290 °C have the potential to cause dose underestimation, although this may be reduced by using larger test-dose irradiations. Our study demonstrates considerable potential in the post-IR IRSL method in providing chronological control in studies relevant to human evolution in the later-Pleistocene.     

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.     

Effects of annealing on TL sensitivity of granitic quartz

A TL sensitivity change can usually be observed after the quartz sample is heated to a high temperature. The change of 110°C TL peak or PTTL was reported to be an increase in many studies. The change of TL sensitivity of other TL peaks, mainly 150 and 375°C, with annealing treatments was demonstrated in this study. Two types of TL sensitivities in granitic quartz were found. One type is the low temperature TL sensitivity (<250°C) which increases with annealing time and temperature. Another type is the high temperature TL sensitivity (>250°C) which usually decreases after annealing. If the TL sensitivity is a measure of the population of associated TL traps, the trap population is a potential geochronometer to date a cooling age of a granite host.     

Phototransferred Thermoluminescence of Dosimetric α-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Crystals Irradiated by a Pulsed Electron Beam

The thermoluminescence (TL) of deep traps of anion-defective alumina monocrystals irradiated by a high-dose (more than 1 kGy) pulsed electron beam (130 keV) is studied. The deep traps in the studied material are classified according to the TL temperature range. It is demonstrated that the phototransferred thermoluminescence (PTTL) in the temperature range of the main TL peak is induced by optical charge migration from deep traps that are emptied at 400–470 and 470–600°C. An anomalous PTTL enhancement in crystals subjected to stepped annealing in the 350–400°C interval is observed. It is demonstrated that this effect may be caused by competing processes of charge transfer that involve deep traps corresponding to the TL peak at 390°C. The applicability of PTTL in the dosimetry of high-dose (1–50 kGy) pulsed electron beams is established.     

Effects of thermally transferred signals in the post-IR IRSL SAR protocol

The recently developed post-IR IRSL SAR protocol is promising to isolate more stable IRSL signals of feldspars. However, the high temperature thermal treatments used will inevitably induce thermally transferred post-IR IRSL₂₉₅ (TT-post-IR IRSL₂₉₅) signal, which would contribute to the measured post-IR IRSL₂₉₅ signal of the test dose and may lead to inaccurate sensitivity correction. In this study, the effects of TT-post-IR IRSL₂₉₅ signal in the post-IR IRSL₂₉₅ SAR protocol are investigated using medium polyminerals from a loess section at Caoxian, northwestern Loess Plateau in China. The sensitivity changes of the IRSL₅₀ and the post-IR IRSL₂₉₅ signals are different from natural cycle to regenerative cycles, which can be attributed to the interference of the TT-post-IR IRSL₂₉₅ signal. Such difference is dependent on the test dose and the post-IR IR stimulation time. The TT-post-IR IRSL₂₉₅ signal is also shown to affect the post-IR IRSL₂₉₅ D_o and D_e values and to cause overestimation of the fading rates. Our study therefore highlights the need of serious consideration on the effects of TT-post-IR IRSL signal when the post-IR IRSL SAR protocol is employed for dating.     

Modelling the optical bleaching of the thermoluminescence of K2YF5:Pr3+

Optical bleaching of the thermoluminescence (TL) curve of K₂YF₅:Pr³⁺ has been observed after optically stimulated luminescence (OSL) readout of pre-irradiated crystals. The traps being responsible for the TL signal are not emptied completely by the optical stimulation. Furthermore, if the illumination time is increased a constant intensity level of the residual TL glow curve is eventually achieved. On the other hand, if the low temperature peak of the glow curve is thermally cleaned, no subsequent OSL is measured. This behavior has been successfully explained by assuming that part of the electrons in the trap being responsible for the low temperature glow peak of K₂YF₅:Pr³⁺ recombine with holes via localized transitions during optical stimulation. During TL all trapped electrons recombine via delocalized transitions. Simulations have been carried out in order to demonstrate the feasibility of the model.     

Characterization of deep energy level defects in α-Al2O3:C using thermally assisted OSL

Commercially available α-Al₂O₃:C powder was studied for deep energy level defects by a newly suggested method using thermally assisted optically stimulated luminescence (TA-OSL) phenomenon. The method involves simultaneous application of continuous wave optically stimulated luminescence (CW-OSL) as well as thermal stimulation up to 400 °C, using a linear heating rate of 4 K/s. By using this method, two well-defined peaks at 121 °C and 232 °C were observed. These TA-OSL peaks have been correlated to two different types of deeper defects which can be bleached at 650 °C and 900 °C respectively on thermal treatment. These deeper defects, having larger thermal trap depth and relatively lower photoionization cross-section at room temperature for stimulation with blue LED (470 nm), are stable up to 500 °C, so they can store absorbed dose information even if the sample is inadvertently exposed to light or temperature. As only a fraction of signal is bleached during TA-OSL readout, multiple readouts could be performed on an exposed sample using this technique. The dose vs TA-OSL response from deep traps of α-Al₂O₃:C was found to be linear up to 10 kGy, thus extending its application for high dose dosimetry. The value of thermally assisted energy (E_A) associated with these traps in α-Al₂O₃:C has been determined to be 0.268 eV and 0.485 eV respectively and the corresponding values of photoionization cross-section at room temperature (25 °C), for optical stimulation with blue light (470 nm), are 5.82 × 10^?20 and 3.70 × 10^?22 cm², respectively. The process of thermally assisted OSL has been formulated analytically as well as theoretically for describing the temperature dependence of optical cross-section and evaluation of thermally assisted energy associated with deep traps.     

Gamma ray induced sensitization of 110°C TL peak in quartz separated from sand

We have investigated the gamma ray induced sensitization of the 110°C TL peak in quartz, separated from sand, in the dose range 30–750 Gy. A pre-dose of 100 Gy followed by annealing at 500°C for 1 h yielded an optimum sensitization factor of 14.2 for a test gamma dose of 0.5 Gy; this factor decreases slowly up to the studied pre-gamma dose of 750 Gy. From ESR studies carried out in the temperature range 25–550°C, the formation of E′₁-centres and their subsequent decay (at temperatures >400°C) have been observed. The released charge carriers (electrons) may lead to elimination of competitors (as a result of their filling up). Thus, the radiation-induced sensitization of the 110°C TL peak could be due to elimination of the competing deep traps.