Tom 40 (2013): Zeszyt 4 (December 2013)
Special Zeszyt Title: Proceedings of the 3rd Asia Pacific Conference on Luminescence and Electron Spin Resonance Dating Okayama, Japan, 2012

The newly developed lexsyg system by Freiberg Instruments is a versatile luminescence reader, suited for research on the luminescence of materials, fundamental research in luminescence dating, but also for routine mass measurements in retrospective dosimetry as well as in dating application. The 80 sample storage wheel is disconnected from the measurement chamber and therefore crosstalk of optical stimulation is absent and cross-irradiation is negligible from the α- and β-sources, which are providing very uniform irradiations, with the latter especially designed for radiofluores-cence (RF) measurement. Optical excitation sources and filter wheels to vary detection wavelengths can be programmed to change at almost any time within measurement sequences, including the auto-mated change of an optional wheel holding up to four different detectors. Thermoluminescence meas-urements and preheating are possible with a versatile heater, which can be programmed for linear or non-linear heating or cooling, as well as holding a temperature constant. Rates as well as durations can be varied, together with individual ramping, staging and cooling for an almost unlimited number of steps. Violet- and IR-lasers, green and blue LED-arrays can be operated in continuous (CW) or modulated mode (linear/non-linear), and optionally for pulsed as well as time resolved luminescence detection. Six arrays of power LEDs allow the simulation of different bleaching regimes (‘solar simu-lator’), while luminescence detection can be achieved by a variety of photomultiplier tubes and by CCD cameras for spatially resolved measurements and luminescence spectra.

The residual doses and sensitivity change for potassium-rich feldspar (K-feldspar) have been studied using the post-infrared infrared stimulated luminescence (pIRIR) and multi-elevated-temperature post-IR IRSL (MET-pIRIR) protocols. Laboratory simulated poorly-bleached and well-bleached samples were those K-feldspar grains bleached using a solar simulator for 10 minutes and 8 hours, respectively. The residual doses rise with stimulation temperature and time. The poorly-bleached sample has larger residual doses than the well-bleached sample, especially at high stimulation temperatures. The high-temperature pIRIR signals contain a large amount of hard-to-bleach signals. A decrease of luminescence sensitivity was observed after conducting a high-temperature-treatment in the measurement cycles. The sensitivity decreases significantly between the first and the second cycle. The extent of decrease in sensitivity shows a clear temperature trend. The higher the stimulation temperature of pIRIR signals is, the larger the sensitivity decreases. This decrease is more severe for the poorly-bleached sample than for the well-bleached sample, and could possibly lead to problems in sensitivity correction.

Cathodoluminescence (CL) spectral analysis has been conducted for luminescent forsterite (olivine) of terrestrial and meteoritic origins. Two emission bands at 3.15 and 2.99 eV in blue region can be assigned to structural defect centres and two emission bands at 1.91 and 1.74 eV in red region to impurity centres of Mn2+ and Cr3+, respectively. These emissions reduce their intensities at higher temperature, suggesting a temperature quenching phenomenon. The activation energy in the quenching process was estimated by a least-square fitting of the Arrhenius plots using integrated intensity of each component as follows; blue emissions at 3.15 eV: 0.08–0.10 eV and at 2.99 eV: 0.09–0.11 eV, red emissions at 1.91 eV: ∼0.01 eV and at 1.74 eV: ∼0.02 eV. The quenching process can be construed by the non-radiative transition by assuming the Mott-Seitz model. The values of activation energies for blue emissions caused by structural defects correspond to the vibration energy of Si-O stretching mode in the lattice, and the values for red emissions caused by Mn and Cr impurity centres to Mg-O vibration energy. It implies that the temperature quenching energy might be transferred as a phonon to the specific lattice vibration.

Cathodoluminescence (CL) of minerals such as quartz and zircon has been extensively studied to be used as an indicator for geodosimetry and geochronometry. There are, however, very few investigations on CL of other rock-forming minerals such as feldspars, regardless of their great scientific interest. This study has sought to clarify the effect of He+ ion implantation and electron irradiation on luminescent emissions by acquiring CL spectra from various types of feldspars including anorthoclase, amazonite and adularia. CL intensities of UV and blue emissions, assigned to Pb2+ and Ti4+ impurity centers respectively, decrease with an increase in radiation dose of He+ ion implantation and electron irradiation time. This may be due to decrease in the luminescence efficiencies by a change of the activation energy or a conversion of the emission center to a non-luminescent center due to an alteration of the energy state. Also, CL spectroscopy of the alkali feldspar revealed an in-crease in the blue and yellow emission intensity assigned to Al-O−-Al/Ti defect and radiation-induced defect centers with the radiation dose and the electron irradiation time. Taken together these results indicate that CL signal should be used for estimation of the α and β radiation doses from natural radionuclides that alkali feldspars have experienced.

Plagioclase feldspar is the major luminescent mineral in meteorites. Thermoluminescence (TL) characteristics, peak temperature (Tm), full width at half maximum (FWHM), ratio of high (HT) to low temperature (LT) peak, and TL sensitivity (TL/dose/mass) to an extent reflect degree of crystallinity of the mineral. The present study explores and establishes a correlation between quantum mechanical anomalous (athermal) fading and structural state by examining TL of individual chondrules. Chondrules were separated using freeze-thaw technique from a single fragment of Dhajala meteorite. The results show large variation in Tm (155−230°C), FWHM (80−210°C) and HT/LT (0.07–0.47) and seem to be positively correlated. TL sensitivity (ranging from 14 to 554 counts/s/Gy/mg) decreases with increasing Tm and FWHM. Large variations in TL parameters (Tm, FWHM, HT/LT, and Sensitivty) suggest that individual chondrules had different degree of crystallization. Thermal annealing experiments suggest that comparatively ordered form of feldspar can be converted to a disordered form by annealing the sample at high temperatures (1000°C) for long time (10 hr) in vacuum (1 mbar pressure) condition and rapidly cooling it. Measured anomalous fading suggest that fading rate increases as the crystal form changes from an ordered state to a disordered state. However, the fading rate becomes nearly negligible for the most disordered feldspars.

The influence of electron-phonon interaction on the shape of the optically stimulated luminescence decay curve of Al2O3:C has been studied using thermally assisted optically stimulated luminescence (TA-OSL). The minimum detectable dose (MDD) of a phosphor depends on the standard deviation of the background signal which affects the signal-to-noise ratio. The standard deviation of the background signal reduces at lower stimulation light intensity while the readout time increases. Further, measurement at higher temperature enhances the OSL signal with faster decay due to the temperature dependence of photo-ionization cross-section. To achieve the same decay constant and more signal, the temperature of measurement was raised. As a result of lowering the stimulation in-tensity at higher temperature (85°C) the overall MDD of α-Al2O3:C was found to improve by 1.8 times. For extension of dose linearity in higher range, deeper traps were studied by simultaneous application of CW-OSL and thermal stimulation up to 400°C, using a linear heating rate of 4K/s. By using this method, two well defined peaks at 121°C and 232°C were observed. These TA-OSL peaks have been correlated with two deeper defects which can be thermally bleached at 650°C and 900°C respectively. These deeper defects are stable up to 500°C, so they can store absorbed dose information even if the sample is inadvertently exposed to light or heat. 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.

Infrared radioluminescence (IRRL) of K-feldspar, detected at peak wavelength of 865 nm, is emerging as a potential geochronometric tool. The present study explores and attempts to optimize the IRRL dating protocols and proposes a revised protocol for estimation of palaeodose. UV light (395 nm; 700 mW/cm2) bleach of 800 s was optimum to remove the trapped charges responsible for IRRL and, reduced the interference of radio-phosphorescence due to prior irradiations. Validation of the proposed protocol was carried out by dose recovery tests on mineral and sediment K-feldspar samples of different provenances. An overestimation in dose recovery was observed and was attributed to difference in sensitivity of natural IRRL and regenerated IRRL. The sensitivity changes were significant and systematic and were documented by repeating bleach-IRRL cycles. Corrections for sensitivity changes between natural and regenerated IRRL, gave reliable results and, have now been included in the proposed dating protocol.

Red sand dunes occur in the coastal plains of south east and west of Tamil Nadu, India between the coordinates of 8°00′ to 9°30′ N; 77°18′ to 79° 00′ E. OSL dating of these sands indicated aggradations between ∼16-9 ka and ∼9-3 ka in the west and east coasts respectively. Dating results from inland red dunes at the foothills of Western Ghats show a break in deposition at ∼6 ka and aggradation since ∼2 ka. The sand aggradations in the west coast occurred during the transition period when SW monsoon in the area was reestablishing. The dunes attained their stability by 9 ka. In the coastal region, the aggradations were controlled by sea level changes and a local recycling of earlier dunes (in the east coast). In the inland areas, the dune building was controlled by sand supply from fluvial sources.

This study investigates the potential of luminescence to date deposits from different fluvial sedimentary environments; namely point bar deposits, sandy and silty channel fills and floodplain sediments. Samples were taken from Holocene (<5 ka) terraces of the Lech and Danube rivers, for which independent age constraint is available through 14C ages, archaeological data and historical maps. OSL-ages were obtained using small aliquots of coarse grain quartz for the majority of samples. Two further samples were dated by the IRSL-signals of polymineral fine grain extracts, as no sufficient number of coarse grains could be extracted from these sediments. In order to detect and ac-count for incomplete bleaching, we used the decision process suggested by Bailey and Arnold [Statistical modelling of single grain quartz De distributions and an assessment of procedures for estimating burial dose. Quaternary Science Reviews 25, 2475–2502, 2006]. Although their model was designed for single grains of quartz, our study shows that it is also applicable to multiple grains of quartz, pro-vided that a low number of luminescent grains is present on one aliquot. Luminescence ages of point bar deposits and a sandy channel fill correspond most closely to the independent age control. In the floodplain, sand-striped floodplain channel deposits were incompletely bleached to a moderate degree, yielding ages with acceptable overestimations, while fine-grained floodplain deposits were worst bleached. One crevasse splay deposit was so severely incompletely bleached that none of the age models was able to yield accurate ages.

Luminescence dating has been applied to volcanogenic outburst flood sediments (Takuma gravel bed) from Aso volcano, Japan, and tephric loess deposits overlying the gravel bed. The poly-mineral fine grains (4–11 μm) from loess deposits were measured with pulsed optically stimulated luminescence (pulsed OSL) and post-IR infrared stimulated luminescence (pIRIR) methods, whereas the Takuma gravel bed containing no quartz, was measured with IRSL and pIRIR methods using sand sized (150–200 μm) plagioclase. The loess deposits date back at least to ∼50 ka by consistent IRSL, pIRIR and pulsed OSL ages from the lowermost part of the loess deposits from one section. The ages obtained from the bottom part of the other loess section are not consistent each other. However, we consider that the pIRIR age (72±6 ka) which showed negligible anomalous fading is most reliable, and regard as a preliminary minimum age of the Takuma gravel bed. The equivalent doses (De) for the plagioclase from the Takuma gravel bed have a narrow distribution and the weighted mean of the three samples yield an age of 89±3 ka. This age is in agreement with the last caldera-forming eruption of Aso volcano (∼87 ka) and it is likely that the pIRIR signal has not been bleached before the deposition. IRSL dating without applying pIRIR using small aliquots was also conducted, however, the IRSL signal shows no clear evidence of an additional bleaching during the event of outburst flood from the caldera lake.

Optically Stimulated Luminescence (OSL) of quartz, with closure temperatures of 30–35°C in conjunction with Apatite Fission Track (AFT; closure temp. ∼120°C) and 40Ar-39Ar (biotite closure temperature ∼350°C), were used to obtain cooling ages from Higher Himalayan crystalline rocks of Western Arunachal Himalaya (WAH). Cooling age data based on OSL, AFT and Ar-Ar thermochronology provide inference on the exhumation — erosion history for three different time intervals over million to thousand year scale.

Steady-state exhumation of ∼0.5 mm/yr was observed during Miocene (>7.2 Ma) till Early Pleistocene (1.8 Ma). Onset of Pleistocene glacial/interglacial conditions from ∼1.8 Ma formed glaciated valleys and rapid erosion with rivers incising deep valleys along their course. Erosion enables midcrustal partial melts to move beneath the weak zone in the valley and causes an erosion-induced tectonic uplift. This resulted in a rapid increase in exhumation rate. The OSL thermochronology results suggest increased erosion over ∼21 ka period from Late Pleistocene (2.5 mm/yr) to Early Holocene (5.5 mm/yr) and these are to be contrasted with pre 1.8 Ma erosion rate of 0.5 mm/yr. Enhanced erosion in the later stage coincides with the periods of deglaciation during Marine Isotope Stages (MIS) 1 and 2. The results of the present study suggest that in the present setting OSL thermochronology informed on the short-term climatic effect on landscape evolution and techniques like the AFT and 40Ar-39Ar provided longer-term exhumation histories.

Although radiocarbon (14C) dating, uranium-series dating, and optically stimulated luminescence (OSL) dating have been conducted for Upper Palaeolithic sites in the Nihewan Basin, northern China, there is room for constructing a detailed chronological framework. In this study, loess sediments collected from two Upper Palaeolithic sites, Youfang site and Hutouliang site, were dated using the single-aliquot regenerative-dose (SAR) OSL protocol. OSL measurements for palaeodoses estimation used fine-grained quartz samples extracted from loess. OSL dating results were obtained as 10–17 ka. These OSL ages were consistent with the related stratigraphy of Palaeolithic sites, archaeological evidence and independent 14C ages.

In this paper, we studied the thermal history of a clay core sample from one leg of a bronze tripod unearthed at Daxinzhuang Site, Shandong, China. The properties of the luminescence signals of quartz depend on the maximum temperature at which the quartz was annealed in the past. We examined the feasibility of measuring the thermoluminescence (TL) sensitivity change of quartz for exploring the firing temperature of archaeological materials. The sensitization factor of the 110°C TL peak (S2/S1) and the ratio of the 210°C TL peak to the 110°C TL peak at different annealing temperatures were utilized to unveil the firing temperature in the clay core sample. The firing temperature of the clay core sample was approximately 700°C–800°C, proving the clay core has been fired. This result proved that the clay core has been fired by human agencies and indicated on the temperature of the clay core in drying and firing given by the foundry workers before the actual casting step.

In the context of human evolution, fossil remains are too valuable to be destroyed and any alteration should be kept to a minimum. The newly developed protocol on fossil fragments has open the gate for ‘virtually’ non-destructive ESR (Electron Spin Resonance) direct dating of human remains. The method allows the separation of unstable and interfering signals that were responsible for large dose underestimation. While a complete investigation of the ESR signal remains a complex task and requires numerous hours of manipulations, a rapid dose assessment protocol can be achieve without compromising the accuracy nor the integrity of the sample. The new protocol should be used for future dating regardless of the possibility of measuring powder.

The variation of electron spin resonance (ESR) signal intensities and thermoluminescence colour images (TLCIs) of quartz was investigated in the present study for various rocks and sediments in Japan, to discuss the possibilities of identifying the sediment provenance. The ESR signal intensity of the E1’ centre in the same grain size in granitic quartz varies from sample to sample, except for that in Quaternary samples of volcanic sediment, which is very low, close to the noise level. It was found that the diagram, ESR intensities of Al versus Ti-Li centre signal intensities, distinguish volcanic from the same grain size in granitic quartz as well as distinguish individual tephra from another. The TLCIs from volcanic quartz and some granitic quartz samples is almost red and that from the rest of granitic and metamudstone quartz is blue as results of TLCIs although the emission intensities are different. Our results suggest that examining the multiple-centre signal intensities of ESR and the TLCIs are effective to identify the source of quartz and to estimate the sediment provenance.

The ESR dating method requires to describe the evolution of the ESR signal intensities vs. increasing gamma doses, then to extrapolate the equivalent dose of radiation received by the sample since its deposition using mathematical fitting. The function classically used to describe the growth curves of ESR aluminium signal in quartz was recently discussed and challenged for Lower Pleistocene sediments. In the present work, some alluvial sediments sampled in Upper Pleistocene fluvial terraces of the Yellow River system (China) permit us to test the application of another extrapolation function (linear + exponential) recently proposed for Lower Pleistocene sediments. The equivalent doses obtained here for the recent deposits of the Yellow River system and the corresponding ages are promising and indicate the potential of ESR to date quartz deposits from Upper Pleistocene times.

The fluvio-lacustrine sequences in the Nihewan Basin, northern China, provide important terrestrial archives about Palaeolithic settlements and, therefore, about early human occupation in high northern latitude in East Asia. Here we present detailed ESR dating of the Donggutuo Palaeolithic site, located in this basin. Four levels A, B, C and E of the Donggutuo archaeological layer yield ESR ages ranging from 1060±129 ka to 1171±132 ka with a mean of 1119±132 ka. The ages are consistent with the paleomagnetic data, which show that the Donggutuo Palaeolithic site lies just below the onset of the Jaramillo normal subchron (0.99–1.07 Ma). Furthermore, our results indicate that the reliable ESR dating range of bleached quartz using Ti-Li centre can be effectively extended to 1100 ka and the Ti-Li centre was zeroed before the last deposition, which requires improvement of the understanding of the bleaching mechanism conditions.

The temporal change in the number of oxygen vacancies in quartz was investigated by ob-serving the E1’ center in the atmospheric depositions collected at two cities in Japan in the recent past. The depositions collected at Fukuoka in March show the ESR intensities being correlated with the sum of the number of the days, in the month, on which Kosa was observed while no such correlation was found in the deposition those collected at Akita but a trend of decrease with time. The present results suggest that the number of oxygen vacancies in quartz might be useful to estimate quantitatively the contribution of the dust originated from China to the atmospheric deposition in Japan.

The Minjiang River terrace along the Longmen Shan fault zone near Wenchuan, at the eastern margin of the Tibetan Plateau, China, provides archives for tectonic activity and quaternary climate change. However, previous studies were not able to provide ages older than 100 ka due to the limitations of dating material or/and methods applied to date the fluvial sediments. In this study, we used the ESR signal of the Ti-Li center in quartz to obtain the ages of four higher terraces (T3–T6). According to the results, the terraces T3 to T6 were formed at 64±19 ka, 101±15 ka, 153±33 ka, and 423±115 ka, respectively. Combined with previous studies, these results indicate that the formations of all terraces correspond to glacial/interglacial transition periods, such as, T1-T5 being correlated to MIS2/1, MIS4/3, MIS5d/5c, and MIS6/5e respectively, while T6 probably to MIS12/11. According to these data, it is found that the average incision rate was significantly higher over the last 150 ka than that previous 100 ka (250 to 150 ka). As both tectonics and climate have affected the formation of these terraces, in addition to the overall uplifting of Tibetan Plateau, the regional uplift due to isostasy would be an additional tectonic factor in the formation of river terraces in the eastern margin of Tibetan plateau.