Underestimation of equivalent dose in single-aliquot optical dating of feldspars caused by preheating

The ability of single-aliquot techniques to recover a known laboratory dose in coarse-grain potassium-rich feldspar separates is tested. It is shown that, for the samples under study, single-aliquot methods underestimate the known dose. It is deduced that this phenomenon is caused by an increase in electron trapping probability as a consequence of heating. The same phenomenon would lead to an underestimation in the equivalent dose in a natural sample. Multiple-aliquot techniques for equivalent dose determination may not suffer from this problem, but are not suitable for samples that might not have been completely bleached at the time of deposition. It is argued that testing for changes in electron trapping probability should become routine practice in the single-aliquot dating of feldspar.     

Reliability of single aliquot regenerative protocol (SAR) for dose estimation in quartz at different burial temperatures: A simulation study

The single aliquot regenerative protocol (SAR) is a well-established technique for estimating naturally acquired radiation doses in quartz. This simulation work examines the reliability of SAR protocol for samples which experienced different ambient temperatures in nature in the range of −10 to 40 °C. The contribution of various experimental variables used in SAR protocols to the accuracy and precision of the method is simulated for different ambient temperatures. Specifically the effects of paleo-dose, test dose, pre-heating temperature and cut-heat temperature on the accuracy of equivalent dose (ED) estimation are simulated by using random combinations of the concentrations of traps and centers using a previously published comprehensive quartz model. The findings suggest that the ambient temperature has a significant bearing on the reliability of natural dose estimation using SAR protocol, especially for ambient temperatures above 0 °C. The main source of these inaccuracies seems to be thermal sensitization of the quartz samples caused by the well-known thermal transfer of holes between luminescence centers in quartz. The simulations suggest that most of this inaccuracy in the dose estimation can be removed by delivering the laboratory doses in pulses (pulsed irradiation procedures).     

The problem of dating quartz 2: Synchrotron generated X-ray excited optical luminescence (XEOL) from quartz

The luminescence emission of quartz is used in optically stimulated luminescence dating (OSL), however the precise origins of the emission are unclear. A suite of quartz samples were analysed using X-ray excited optical luminescence (XEOL). Radiation dose effects were observed whereby the UV emissions (3.8 and 3.4 eV) were depleted to the benefit of the red emission (1.9–2.0 eV). Samples were excited at ∼7 keV. Understanding why some quartz emit light more brightly than others will increase the efficiency and precision of OSL analyses.     

Testing the reliability of ESR dating of optically exposed buried quartz sediments

Optical dating of quartz by optically stimulated luminescence has a time range that is generally less than about 500 ka, due to relatively rapid saturation of the available luminescence defects in quartz. We test here a new method, electron spin resonance (ESR) optical dating of quartz, in which radiation-sensitive defects at aluminum and titanium atoms on silicon sites give rise to signals which can only be detected near liquid nitrogen temperature and which have a much higher capacity to absorb radiation dose before saturating than optical luminescence-detected signals. Our results show this method yields agreement with independent age control out to about 2.5 million years, extending here the dating range of optically exposed quartz in sediments in along-shore sediments (aeolian and waterlain) by a factor of about 5. Three sites in along-shore lacustrine and marine aeolian environments yielded very good agreement with independent age control. Details of single saturating exponential fitting in relation to agreement with expected burial doses and annealing of Al and Ti signals provide additional data to consider the best approaches to the dating method. Furthermore, we propose a new criterion for ESR optical dating: both the Al signal and Ti signal ages must agree to insure accurate burial ages. Moreover, when Al signal ages are lower than Ti signal ages, then the Al signal may be taken as the minimum burial age.     

Investigations of the performance of quartz single aliquot DE determination procedures

Over the past few years a variety of equivalent dose (D_E) determination techniques for quartz, which are truly single aliquot-based, have been proposed. Such methods avoid the need for inter-aliquot normalisation, and provide considerable improvements in the precision of equivalent dose (D_E) estimates. Much of the research leading to these developments have been based on detailed investigations of a few samples, primarily from Australia. All ’protocols’ developed have performed impressively. It is necessary, however, to verify the consistency of the single aliquot D_E determination methods on a wide range of samples before they can be considered as prescribed or standard. We have analysed approximately 100 samples from a range of sedimentary environments and geological provinces in an attempt to confirm the robustness of the single aliquot techniques. Up to 65% of samples measured in our laboratory were not suited to analysis via application of single aliquot additive dose (SAAD) procedures. This relates to a range of factors, including lack of sample sensitivity and dose dependent sensitivity changes. Furthermore, we have observed some problems in dating young sediments using single aliquot regeneration (SAR) methods. Critically, we observe that sample to sample variability on quartz luminescence (thermally- and optically-stimulated) behaviour is considerable, and many samples are found to exhibit behaviour which contrasts greatly from that described in recent phenomenological studies.     

A comparison of single and multiple aliquot TT-OSL data sets for sand-sized quartz from the Arabian Peninsula

The quartz OSL signal from dune sands from Saudi Arabia and Oman start to saturate at doses of about 100 Gy. In order to try to date dune sands with greater expected doses, a previously published, single-aliquot, regenerative-dose protocol (SAR) for thermally-transferred optically stimulated luminescence (TT-OSL) was tested. Dose recovery tests, recycling and recuperation ratios showed robust functioning and dose response curves demonstrated the potential to extend the dose range to beyond 600 Gy. Multiple aliquot additive dose (MAAD) TT-OSL protocols were used to test for sensitivity changes in the SAR TT-OSL protocol up to doses of 1200 Gy. A strong dose dependent deviation of the SAR TT-OSL relative to the MAAD TT-OSL dose response is observed. Comparison of the TT-OSL and OSL sensitivity data obtained from the MAAD and SAR data sets shows a lack of proportionality between TT-OSL and OSL for the SAR data which will result in a problem when SAR dose response curves are constructed using many regeneration points with doses above 300 Gy.     

Luminescent, optical and color properties of natural rose quartz

Rose quartz is an interesting mineral with numerous impurities that have been studied by scanning electron microscopy (SEM), X-ray fluorescence (XRF), X-ray diffraction (XRD), cathodoluminescence (CL), ion beam luminescence (IBL), radioluminescence (RL), thermoluminescence (TL) and optical absorption (OA). After HF etching, rose quartz from Oliva de Plasencia (Caceres, Spain) shows under SEM the presence of other silicate phases such as dumortierite $[{\mathrm{Al}}_{6.5-7}({\mathrm{BO}}_3)({\mathrm{SiO}}_4{)}_3(\mathrm{O},\mathrm{OH}{)}_3]$. The OA spectrum of rose quartz suggests that these inclusions are the cause of coloration of rose quartz. The luminescence (CL, IBL, RL, TL) spectra behavior, at both room temperature and lower, confirms that the $\sim 340\mathrm{nm}$ emission could be associated with Si–O strain structures, including non-bridging oxygen or silicon vacancy–hole centers; the observed $\sim 400\mathrm{nm}$ emission could be associated with recombination of a hole trapped adjacent to a substitutional, charge-compensated aluminum alkali ion center; the $\sim 500\mathrm{nm}$ emission could be associated with substitutional ${\mathrm{Al}}^{3+}$ and the $\sim 700\mathrm{nm}$ peak could be associated with ${\mathrm{Fe}}^{3+}$ point defects in ${\mathrm{Si}}^{4+}$ sites. These results suggest that, while defect properties of rose quartz are not greatly dissimilar to those of purer forms of quartz and silica, further research seems necessary to determine criteria for the evolution of the newly-formed self-organized microstructures in the rose quartz lattice under irradiation.     

A new irradiated quartz for beta source calibration

For luminescence dating to be an accurate absolute dating technique it is very important that we are able to deliver absolutely known radiation doses in the laboratory. This is normally done using a radiation source (alpha, beta, X-ray) calibrated against an absolutely known reference source. Many laboratories have used the various different batches of Risø calibration quartz for the calibration of beta and X-ray sources, but these have been largely undescribed. Here we describe in detail the preparation and luminescence characteristics of a new quartz standard, based on a North Sea beach sand collected from south-western Denmark (Rømø). Two grain sizes (4–11 μm and 180–250 μm) have been examined in detail. These were pre-treated (annealed, dosed and annealed again) to sensitise and stabilise the luminescence signals before being given an absolutely known gamma dose from a point ¹³⁷Cs source in scatter-free geometry. The luminescence characteristics are described; the very intense blue-light stimulated signal is dominated by the fast OSL component and the IR-stimulated signal is negligible. The material is shown to be suitable for measurement using SAR, and the dose recovery ratio is indistinguishable from unity with a standard deviation of <2% for multi-grain aliquots. The material is also shown to be suitable for single-grain calibration, with >80% of the grains giving a useful signal. Although there is an unexplained dispersion in our calibration data of ∼3% (which we cannot attribute to instrument variability), we nevertheless conclude that this material is very suitable for transferring absolute known doses from a standardised gamma source to in-built irradiation sources.     

Extending the age range of optical dating using single ‘supergrains’ of quartz

Luminescence dating methods have been used to obtain reliable age estimates for quartz sediments deposited within the last 500 ka, but it has proven difficult to extend the age range much beyond this limit. Here we report the results of a study of individual quartz grains from Australian sedimentary deposits that range in age from 250 to 950 ka. A small number of the grains examined are strongly luminescent and saturate at unusually high doses. These ‘supergrains’ may permit reliable age determination to 1 Ma, and possibly beyond. Some other grains are in, or close to, dose-saturation, so that only minimum age estimates may be obtained. Most of the grains examined are very weakly luminescent and have palaeodoses much less than expected, while the palaeodoses of some grains cannot be estimated because of anomalous dose–response characteristics. We offer some possible explanations for the behaviour of aberrant grains.     

Palaeodose underestimates caused by extended-duration preheats in the optical dating of quartz

An optical dating study of some quartzose sediments from northern and southern Australia, north Africa and north-western Europe has revealed that palaeodose (P) underestimates of 10–40% are obtained when an extended-duration preheat of 160°C for 16 h is used. For these samples in the 0–60 ka age range, a preheat of 220°C for 5 min produces the correct P, as inferred from the concordance with thermoluminescence (TL) palaeodose determinations on the same sedimentary sample or on burnt flint. Independent support for use of the 220°C preheat is given by the agreement between optical ages younger than 30 ka and ¹⁴C age determinations on associated charcoal. The deleterious effect of the 160°C preheat is illustrated by growth curves of optically stimulated luminescence (OSL) vs added dose. These curves show that the 160°C preheat induces a dose-dependent increase in sample sensitivity, which may be related to activation of the pre-dose mechanism. The 160°C preheat also causes low-dose supralinearity, although the supralinearity correction is insufficient to reduce significantly the degree of P underestimation. A normalization method based on preheat-induced sensitivity changes of the 110°C TL peak, albeit limited by saturation effects, warrants further investigation.     

Growth and characteristics of some new varieties of coloured quartz single crystals

Abstract

Methods for the hydrothermal synthesis of four new coloured varieties of quartz have been developed. Two of these varieties are very rare in nature. They are a bi-coloured amethyst-citrine quartz (ametrine) and a phosphorous-bearing low-temperature pink quartz. The other two varieties have no natural counterparts. They are a pink-violet Ni-bearing quartz, and a Cu-bearing quartz which resembles aventurine. The principal conditions for producing these varieties of quartz single crystals are described.     

A method for water well regeneration based on shock waves and ultrasound

The regeneration of water wells is an urgent problem nowadays, when drilling of new wells becomes more and more expensive. Formation damage leads to a reduction of the formation's permeability and/or pore volume which in turn inhibits the ability of the water to flow from the reservoir formation into the wellbore. A new technology that uses high-power ultrasound to remove formation damage of water wells has been developed. The effectiveness of regeneration of wells can be enhanced if ultrasound and shockwaves are used during the same treatment. It was shown by computer modelling, that the two methods have different depths of impact. Whereas the ultrasonic method has a strong impact on the area of the filter tube, the impact of the shock waves is focused on the gavel pack, the wall of the well and the adjacent aquifer. A shockwave treatment, which is normally more effective due to larger impact zone, needs to be followed by ultrasonic treatment in order to facilitate the removal of the detached deposits. These theoretical assumptions were confirmed by field tests on two wells. The use of the method leaded to an increase of the production by 40% and 109% respectively.     

Estimating the parameters of traps in quartz by the variable energy of stimulation optically stimulated luminescence (VES-OSL) method

Optical-cross section that is a trap parameter estimated from the measurements of optically stimulated luminescence (OSL) is not a uniquely determined physical quantity. It depends not only on temperature and the energy of stimulation light but also, in the simplest case, on the optical depth of trap, the frequency of vibration mode and on the Huang-Rhys factor, i.e. the average number of phonons involved in the process of optical excitation of electrons from trap to conduction band. Conventional OSL measurement techniques do not enable to determine directly these parameters but they could be estimated by applying the variable energy of stimulation optically stimulated luminescence (VES-OSL) method. Recently it was put in to practice and the first VES-OSL curves were presented. In this study the outcomes of VES-OSL experiments are presented together with the first attempt of direct estimating the optical depth of traps active in OSL process in quartz.     

Study of the 110°C TL peak sensitivity in optical dating of quartz

As the 110°C TL emission in quartz uses the same luminescence centers as the OSL emission, the 110°C TL signal from a test dose may be used to monitor the OSL sensitivity change. It is thus important to study the relationship between the 110°C TL peak and the OSL sensitivity in studies related to optical dating from quartz. We have conducted a series of experiments using sedimentary quartz, where the annealing temperatures were varied between 260 and 1000°C before the measurement of OSL and 110°C TL sensitivities. Another series of experiments on two sedimentary quartz samples investigated the 110°C TL peak and OSL dose-dependent sensitivity change after different annealing temperatures. In these experiments, the 110°C TL and OSL signals from the test dose are shown to have similar sensitization characteristics: the 110°C TL sensitivity change is proportional to the OSL sensitivity change if the annealing temperature is lower than 500°C. It is concluded that the 110°C TL signal can be used to correct the OSL sensitivity change in the single-aliquot additive-dose protocol.     

Studies on the optical and dielectric properties of a zinc thiourea chloride NLO single crystal

Single crystals of a nonlinear optical material, zinc thiourea chloride were grown by the slow evaporation technique. The crystal structure and lattice parameters of the grown crystal were determined by the single crystal X-ray diffraction studies. The single crystal XRD revealed that the material crystallized in a orthorhombic crystal system. Optical studies were carried out and it was found that the tendency of transmission observed from the specimen, with respect to the wavelength of light, is practically more suitable for opto-electronic applications. The optical band gap is found to be 4.30 eV. Optical constants such as the band gap, refractive index, reflectance, extinction coefficient and real (?_r) and imaginary (?_i) components of the dielectric constant and electric susceptibility were determined from the UV–vis–NIR spectrum. The dielectric constant and dielectric loss of zinc thiourea chloride were measured in the different frequency range from 50 Hz to 5 MHz at different temperatures. Further, electronic properties, such as valence electron plasma energy, Penn gap, Fermi energy and electronic polarizability of the grown crystal have been estimated.     

Cleaving of solid single mode polymer optical fiber for strain sensor applications

Single mode polymer optical fibers (smPOFs) can be applied for measuring large strains in numerous applications, such as civil engineering infrastructure assessment and health monitoring. Because of the large light attenuation of solid smPOFs, small lengths of the fiber would need to be coupled to silica optical fibers (SOFs) for practical applications of the smPOF as a strain sensor. This coupling requires smooth cleaving of the smPOFs. In this work, several cleaving techniques previously demonstrated to provide smooth cross-sections of multimode POFs were applied to the smPOF. From these techniques, hot-knife cutting was determined to be a feasible method for cleaving when the blade was heated to 80 °C and the smPOF heated in the range of 30 °C to 40 °C. In addition, focused ion beam machining which produces high-precision cleaves of the solid smPOF cross-section, was performed to set a bench mark and thus evaluate the quality of cleaving from other methods used in this study.