Optical dating of single sand-sized grains of quartz: sources of variability

Optically stimulated luminescence (OSL) measurements have been made of over 3000 sand-sized grains of quartz. Analysis at this scale highlights the variability in the luminescence sensitivity and the dose saturation characteristics of individual quartz grains. Using a new instrument capable of measuring single grains it is feasible to routinely measure the equivalent dose from many hundreds of grains from each sample. Analysis of such datasets requires assessment of the uncertainties on each equivalent dose since these may vary significantly. This paper assesses the significance of signal intensity, dose saturation characteristics and instrument uncertainty in equivalent dose calculation.     

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.     

Conduction transients using a lagrangian formulation. Part I: Transients modified by their self space-charge

The problem of space-charge-limited current transients for a single species is set up and solved using a Lagrangian reference frame approach. Arbitrary boundary values are allowed for the electric field rather than a simple ohmic condition, and the electrodes are considered to be blocking to injection. A physical realization of the situation would be the motion of a low-mobility species produced by ionizing radiation in an insulator after a more mobile oppositely charged carrier has left the sample.     

Behavioural studies of stimulated luminescence from feldspars

Since the work of Mejdahl in the mid-1980s feldspars have been used widely for palaeodosimetry. They have proved particularly popular because of the technical ease with which an optically stimulated luminescence signal can be obtained, and the potential for their use in dating over a wider time range than quartz. However, while the use of infrared stimulated lminescence has been a great success, the realisation of the potential for dating over a wide time range has been hampered by a series of behavioural problems, in particular concerned with the stability of the luminescence signal. This paper surveys the current state of knowledge of a range of aspects of the stimulated luminescence behaviour of feldspar. Particular attention is paid to the thermal and optical properties of the thermoluminescence (TL) and optically stimulated luminescence (OSL) signals from feldspars since these are of greatest relevance to their use as palaeodosimeters. Results obtained from well-characterised museum specimens demonstrate the variety of responses that are seen from different types of feldspar, particularly in their TL behaviour. Less variation is seen in their OSL response. In contrast, the response of potassium-rich feldspars separated from Quaternary sediments tends to be very consistent when many grains are analysed simultaneously, suggesting that averaging of the signal simplifies the behaviour of the system.     

Reproducibility of optically stimulated luminescence measurements from single grains of Al2O3:C and annealed quartz

We have measured some aspects concerning the performance of a new instrument for the measurement of optically stimulated luminescence (OSL) from single sand-sized grains. The instrument uses a solid-state laser to stimulate OSL from each grain individually. These grains are placed in a regular grid of nine-by-nine holes, which are drilled in the sample disc. We report on tests carried out to determine the precision with which the laser beam can be directed at individual grains in these holes. Single grains of aluminium oxide (Al₂O₃:C) (90–180 μm) and annealed quartz (90–120 μm) were used to test the reproducibility with which the OSL signal can be measured. These experiments suggest that the laser beam can be positioned to within 30 μm and that the reproducibility of OSL measurement is 3.5% on an average.     

The fast ratio: A rapid measure for testing the dominance of the fast component in the initial OSL signal from quartz

The signal from the fast component is usually considered preferable for quartz optically stimulated luminescence (OSL) dating, however its presence in a continuous wave (CW) OSL signal is often assumed, rather than verified. This paper presents an objective measure (termed the fast ratio) for testing the dominance of the fast component in the initial part of a quartz OSL signal. The ratio is based upon the photo ionisation cross-sections of the fast and medium components and the power of the measurement equipment used to record the OSL signal, and it compares parts of the OSL signal selected to represent the fast and medium components. The ability of the fast ratio to distinguish between samples whose CW-OSL signal is dominated by the fast and non-fast components is demonstrated by comparing the fast ratio with the contribution of the fast component calculated from curve deconvolution of measured OSL signals and from simulated data. The ratio offers a rapid method for screening a large number of OSL signals obtained for individual equivalent dose estimates, it can be calculated and applied as easily as other routine screening methods, and is transferrable between different aliquots, samples and measurement equipment.     

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.     

Excitation and emission spectrometry of stimulated luminescence from quartz and feldspars

A new scanning monochromator was designed to investigate the wavelength-resolved luminescence excitation and emission characteristics of quartz and feldspar samples; results are presented, together with detailed measurements of the thermal activation energies required for luminescence stimulation in feldspar over the wavelength range 400–1000 nm. When coupled to automated dating equipment, we demonstrate that optical characteristics of samples selected for dating can be routinely measured, or more detailed analysis of physical processes can be made.     

Developing a single-aliquot protocol for measuring equivalent dose in biogenic carbonates

Exploiting biogenic carbonates as thermoluminescence dosimeters requires an understanding of trap kinetics and an appropriate sequence with which to measure equivalent dose. The trap kinetics of two high temperature peaks (peaks II and III) from calcitic snail opercula have been investigated resulting in the calculation of lifetimes of 7.4 × 10⁷ and 1.4 × 10¹¹ years for the two peaks respectively. Two measurement sequences, based upon changes in the application and measurement of a test dose, have been applied to peaks II and III, and though both methods were equally successful in dose recovery and production of a dose response curve some differences were observed. Primarily, the use of method 1 lead to dose dependant sensitivity change implying competition effects occurring during irradiation; method 2 did not experience this phenomenon. As a consequence method 2 was chosen as the most appropriate protocol for single-aliquot dating of this material.When assessing the TL behaviour of the two peaks, peak II performed poorly in dose recovery experiments recovering a dose 60–100% larger than that applied. Disproportionate growth of peak II in response to a beta dose applied prior to measurement, compared to growth following regeneration doses indicated that peak II was not suitable for use in single-aliquot protocols. However, dose recovery results for peak III were all within errors of unity of the given dose, and peak III was therefore chosen as the most appropriate peak for TL dosimetry in these single-aliquot procedures. The lifetime of charge in peak III is sufficient to date over many millions of years, and furthermore using the chosen method 2 the dose response curve has a D₀ of 3,250 ± 163 Gy allowing dating to over 3 million years.     

A new method for the analysis of infrared stimulated luminescence data from potassium feldspars

A new method is described for the analysis of high precision pulse annealing data obtained using IRSL measurements on potassium feldstars using a Risø reader. Presdenting the data as the percentage of the signal lost per annealing phase permits more detailed comparisons to be made between samples. In addition, it is possible to directly compare the temperatures at which the TL and IRSL signals are released, thus giving information about the relationship between them. This method of analysis is applied to pulse annealing data for natural, irradiated, preheated and IR bleached aliquots.