Red luminescence from potassium feldspar for dating applications: a study of some properties relevant for dating

Aspects of the red thermoluminescence (RTL) and IR (833±5 nm) stimulated red (λ_emission=600–750 nm) luminescence (orange-red IRSL) of potassium feldspar from different origins are described. Anomalous fading of RTL (300–500°C) from a selection of potassium feldspar samples was tested. High temperature RTL (300–450°C) exhibits less anomalous fading in comparison to UV luminescence, for the samples under study. The result supports the contention of Zink and Visocekas (1997) that the red TL emission from feldspar does not fade. It was found that RTL is bleachable due to IR exposure, and the relationship between RTL lost and orange-red IRSL produced is linear. It is shown that around one third of the trapped charge responsible for the orange-red IRSL signal gives rise to an RTL signal, indicating that some traps and luminescence centres are shared for RTL and orange-red IRSL.

Specific characteristics of orange-red IRSL from feldspar were identified. It was found that the orange-red IRSL decay curve is bleachable by IR and daylight and can be described by the sum of three exponential components. Orange-red IRSL fading was tested. Short-term storage tests (up to 2 weeks) showed no fading. Longer-term (ca. months) storage of orange-red IRSL do in fact indicate fading, though at levels considerably lower than for the UV emission. The contradictory result is possibly due to the detection wavelength. As such, it is highly likely that the long-term fading experiment is strongly influenced by the feldspar emission centred at ca. 570 nm, which exhibits anomalous fading, while the short-term fading experiment is more greatly influenced by the far red emission centred at ca. 710 nm that in comparison to UV emission shows no or less fading.     

Na-rich feldspar as a luminescence dosimeter in infrared stimulated luminescence (IRSL) dating

One of the challenges in dating rock surfaces is the choice of the luminescence mineral. Although quartz is the preferred dosimeter in sediment dating, it is often not sufficiently sensitive when extracted from solid rocks. The intensity of signals from feldspars tends to be much less dependent on geological origin and erosion history, but the dosimetry of K-rich feldspar grains extracted from rocks is complicated because the internal dose rate is very dependent on the original feldspar grain size. The in situ grain size information is lost during the crushing process used to separate the grains for measurement. This latter problem does not apply to Na-rich feldspar because of the absence of internal radioactivity.The potential application of Na-rich feldspar as a luminescence dosimeter for the IRSL dating of rock surfaces is investigated using a variety of sediment samples from different geological settings for which independent age control is available. The blue and yellow luminescence emissions are measured for IR stimulation at 50 °C (IR₅₀), and post-IR IR stimulation at 290 °C (pIRIR₂₉₀). Thermal stability experiments imply that the corresponding signals in both emissions have comparable thermal stabilities and that all signals have similar recombination kinetics and are thermally stable over geological timescales. The IR₅₀ doses measured using blue and yellow emissions are similar to or lower than quartz doses while pIRIR₂₉₀ blue doses are higher than those from yellow emission and quartz doses. The fading rates measured for the IR₅₀ signals are ∼3%/decade larger than those measured for the pIRIR₂₉₀ signals in both yellow and blue emissions. Furthermore the average fading rates of both yellow signals are ∼3%/decade higher than the corresponding fading rates of the blue signals. However, there is no detectable correlation between fading rates and the measured D_e values. The residual doses measured from the laboratory-bleached samples and a modern analogue suggest that the IR₅₀ signals in both blue and yellow emissions bleach to the same degree, as do the corresponding pIRIR₂₉₀ signals, and that there is no significant naturally-unbleachable residual dose observed using these signals. Neither anomalous fading nor incomplete bleaching explains the observed dose discrepancy between the two emissions. Eight uncorrected and fading-corrected ages are calculated for each sample based on all four signals, using the dose rate relevant to Na-rich feldspar extracts (i.e. ∼3% K). The IR₅₀ and pIRIR₂₉₀ blue ages were also calculated assuming a dose rate based on 12.5% internal K (i.e. assuming that the blue signals were mainly derived from contamination by K-rich feldspar). The latter pIRIR₂₉₀ blue ages are in agreement with the expected age control, raising the possibility that this signal originates mainly from K-rich feldspar contamination in our Na-rich fractions, and thus is not so useful in the luminescence dating of rock surfaces. On the other hand, the pIRIR₂₉₀ fading-corrected ages based on the yellow emission are consistent with the independent age controls; higher preheat and stimulation temperatures may result in more stable yellow signals from Na-rich feldspar extracts from rocks, and so reduce the size of the fading correction. We conclude that, because this signal avoids the dosimetry difficulties of K-rich feldspar extracts, it has considerable potential in the IRSL dating of rock surfaces.     

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.     

Radioluminescence dating: the IR emission of feldspar

A new luminescence reader for radioluminescence (RL) measurements is presented. The system allows detection of RL emissions in the near infrared region (IR). Basic bleaching properties of the IR-RL emission of feldspars are investigated. Sunlight-bleaching experiments as a test for sensitivity changes are presented. IR-bleaching experiments were carried out to obtain information about the underlying physical processes of the IR-RL emission.     

The fadia method: a new approach in luminescence dating using the analysis of single feldspar grains

The fadia method has been recently introduced in luminescence as one that may potentially resolve the problem of anomalous fading and age shortfalls in IRSL dating of sediments. This method takes advantage of the differential fading rates of single feldspar grains and allows one to extrapolate to zero fading. This paper describes step by step the protocol used in the Montréal laboratory. The application of the method is shown to be hampered by the occurrence of faintly luminescent feldspar minerals, and/or unbleached grains in the dated sediment samples.     

Probing luminescence centers in Na rich feldspar

In contrast to the detailed investigations on the dosimetric electron trap in feldspar only little has been done to understand the luminescence centers. We use a comparison of multiple spectroscopic techniques, site selective photoluminescence spectroscopy and time resolved measurements to further our understanding of the luminescence mechanisms and recombination sites, in a sample of Na rich plagioclase feldspar (oligoclase). Both the UV and violet–blue emissions show resonant excitations arising from a distribution of energy levels. We propose, contrary to the general understanding, that the green emission may not arise from Mn²⁺ in our sample and that photoionisation of this centre may be possible by excitation to the band tail states. The deep red emission is tied to the Fe³⁺, and the exponential rise in the UV excitation efficiency of this centre is discussed in the context of the band-tail model.     

Spectral information from minerals relevant for luminescence dating

The paper reviews basic spectral features of luminescence from minerals used in dating and allied research. Luminescence production is a result of multiple interactions within the imperfect crystal lattice and spectral information is not limited to the emission of light. Results of spectral investigations of luminescence emission during thermal stimulation (TL) or optical stimulation (OSL) form the main part of the paper. However, information on luminescence excitation and light absorption spectroscopy is also presented and possible links between luminescence production in minerals and particular lattice defects are considered. Quartz and feldspars, the most commonly used minerals, receive special attention, but the review includes other materials such as polymineral fine-grained fractions from sediments, zircon, calcite and other salts (halite, sulfate), meteorites, flint, volcanic materials (obsidian, tephra), ceramics and metallurgical slags. Although a wide range of different luminescence emission wavebands occur, it can be shown that certain emissions dominate in particular materials. Basic dosimetric properties are often known just for single emission wavebands of a particular mineral, and are listed in this case. The paper also aims to provide a starting point and inspiration for the study of other TL and OSL emissions, with particular regard to their potential and suitability for dating and related dosimetry tasks. These investigations, involving palaeodose determination based on an emission waveband with known characteristics, need careful separation of the particular emission peak, which may be influenced by its behaviour during the dating procedure (sample preparation, irradiation, preheat treatments, luminescence measurements, etc.). Spectral information available in this context and some technical remarks on the experimental conditions will be given to pave the way for conventional TL or OSL measurements in luminescence dating and dosimetry using natural or semi-natural materials.     

Some aspects of single-grain luminescence dating

Single-grain methods of luminescence dating have been developed in order to circumvent problems of variability among aliquots of the sample being dated. Sufficient single grains must be separated in order to make an appropriate interpretation of the variability among such grains. We describe an automated apparatus for sorting grains for routine age determinations by green light stimulation. The sorted grains are then available for study of their collective luminescence physics characteristics. Examples are given of statistical frequency functions of grain brightness obtained with the apparatus and their interpretation. These frequency functions are lognormal or similar, covering up to four orders of magnitude, with consequent implications for luminescence dating application.     

Steps towards surface dating using luminescence

Whereas luminescence dating applications usually avoid gradients and therefore surfaces, this study explores the requirements and possibilities of dating surfaces using infrared stimulated luminescence. The basic prerequisite for dating applications is a dose-dependent, bleachable and stable luminescence signal. It was found to be fulfilled for crushed granite rock material. Depth profiles below polished surfaces of granites indicate that a well bleached layer below the actual surface solely contributes to the infrared stimulated luminescence signal. A new measurement device, designed for in situ surface dating applications, is presented along with first experimental results.     

Sampling pottery in luminescence dating studies

A programme of dating pottery from Later Prehistoric sites in Britain revealed that pottery sampled from large features such as enclosure ditches is likely to be residual, i.e. not contemporary with the infilling of the feature. This is important since in luminescence dating such features are often preferred due to the simplification of the dosimetry. Dates obtained for the pottery from smaller contexts, however, were clustered and in agreement with the expected date. In the light of these findings, it is recommended that in situations where the purpose of dating the pottery is to date the feature, pottery be sampled from smaller, shorter-lived contexts. This introduces some complications in the dosimetry, but a simple means of determining the gamma dose rate is presented.     

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.     

Sediment dating by luminescence: a review

In the present article we review applications of luminescence methods for the determination of the age of sediments for Quaternary Earth science. “Sediment” is taken to include any mineral particles transported by wind, water and/or ice and subsequently deposited. Methodology is not discussed per se but appears in context. The emphasis is on recent work and is illustrative rather than exhaustive. Applications in archaeology are mentioned only briefly. Successful dating requires that the luminescence signal has been zeroed by sunlight at the time the sediment was laid down. Dune sands and loess transported in full daylight usually satisfy this condition and have been dated by both traditional thermoluminescence and by optical methods. Optical dating is advantageous for less well-bleached sediments, such as are found in colder climates and those laid down by fluvial and glacial processes, although the prospects for dating the latter are shown to be poor. Among less common contexts are volcanic eruptions, earthquake faults and tsunami deposits. The dating of very young sediments, less than 2 ka, is demonstrated and the factors limiting the dating of very old sediments, 500 ka to 1 Ma, are discussed. Validation of any dating method by comparison with other methods is necessary; luminescence ages have been successfully compared with ages obtained by, for example, ¹⁴C, U–Th series and δ¹⁸O isotope ratios. The most difficult problems encountered in dating quartz, feldspars and undifferentiated fine grain mixtures include: anomalous fading (which leads to underestimates of age), incomplete zeroing (which gives overestimates) and sample inhomogeneity. Methods devised to minimise these effects include preheating regimes, selection of observing wavelengths and of stimulating wavelengths for optical dating, the use of single aliquot and single grain measurements. The use of appropriate data analysis procedures is also important. Advice on current best practice on procedures for obtaining reliable ages is offered and, in all applications, there are suggestions as to where further research might be directed.     

Cross-talk during single grain optically stimulated luminescence measurements of quartz and feldspar

Focussed laser systems designed to measure the optically stimulated luminescence (OSL) signals from individual sand sized mineral grains are now widely used. One system that is commonly used can hold up to 100 grains on a 9.8 mm diameter aluminium disc, and can use either a green or infrared (IR) laser for optical stimulation. The grains are held in holes drilled into the disc surface, and the spacing between the edges of adjacent holes is only 300 μm. Focussing of the laser is essential to prevent inadvertent optical stimulation of adjacent grains, but no measurements have previously been made to determine the extent of cross-talk. Measurements on two systems show that the maximum cross-talk for an adjacent position is 0.22%, but typically the value is 0.04% for the green laser and 0.08% for the IR laser. This magnitude of cross-talk is unlikely to have a significant impact on continuous wave OSL measurements where the period of optical stimulation tends to be short, but may be important in linearly modulated OSL measurements where long periods of stimulation are sometimes used to characterise slow components of the OSL signal.     

Identifying well-bleached quartz using the different bleaching rates of quartz and feldspar luminescence signals

When dating older sedimentary deposits using quartz, there are no unambiguous methods for identifying the presence of incomplete bleaching. Current statistical analysis of dose distributions depends entirely on the assumption that incomplete bleaching and mixing are the main causes of any excess dispersion in the distribution; the only existing way to test this assumption is using independent age control. Here we suggest a new approach to this question, based on the differential bleaching rates of quartz and feldspar luminescence signals. We first present data that confirm the differences in relative bleaching rates of quartz optically stimulated luminescence (OSL) and feldspar luminescence stimulated at 50 °C by infrared light (IR₅₀) and feldspar luminescence stimulated at 290 °C by infrared light after a stimulation at 50 °C (pIRIR₂₉₀), and use recently deposited samples to determine the likely significance of the difficult-to-bleach residual feldspar signals in non-aeolian samples. For a set of mainly Late Pleistocene non-aeolian sediments, large aliquot quartz doses are then used to predict feldspar doses (based on a knowledge of the sample dose rates). The differences between observed and predicted feldspar doses as a function of the quartz dose, combined with a conservative assumption concerning the relative feldspar and quartz residual signals after natural bleaching prior to deposition, are used to identify those samples for which the quartz is very likely to be well bleached (20 out of 24). Two of these apparently well-bleached samples are then examined using single-grain quartz dose distributions; one of these is consistent with the well-bleached hypothesis, and one indicates poor bleaching or a multi-component mixture. However, independent age control makes it clear that the large aliquot data are more likely to be correct. We conclude that a comparison of quartz and feldspar doses provides a useful independent method for identifying well-bleached quartz samples, and that it is unwise to apply statistical models to dose distributions without clear evidence for the physical origins of the distributions.     

A practical correction for sensitivity change in thermoluminescence multi-aliquot-regeneration dating of feldspar dominated fine grain loess

Multi-aliquot (MA) thermoluminescence (TL) has been used little since the advent of modern single-aliquot-regenerative-dose (SAR) sediment dating methods for both quartz and feldspar. However, for dating unheated feldspar-bearing sediments older than 100–200 ka, MA TL can still be useful. To improve precision in burial-dose estimation from TL, a post-bleaching regenerative-dose procedure is beneficial. However, the long-known regenerative-dose TL sensitivity changes cause significant age under-estimation in such MA TL. Here a practical procedure is demonstrated to correct for this post-bleaching sensitivity change. Two samples of fine grain, polymineral loess having independent ages of ∼130 ka and ∼350 ka are employed with the use of the SLIDE (combined additive-dose and regenerative-dose responses) procedure to show that not only accuracy but improved precision can be attained with use of this practical procedure. The procedure employs an operational definition of laboratory-dose sensitivity change with respect to a second-glow TL signal, and corrects for the sensitivity change as a function of laboratory dose and of glowcurve temperature.     

Quartz fast component opticallystimulated luminescence: Towards routine extraction for dating applications

Using an uncontaminated fast component is a key for improving the reliability of quartz OSL dating for many deposits. So far no approach to extract the fast component of quartz OSL has routinely been adopted for dating practice. Key challenges for extracting fast components are (1) the difficulty of finding a unique solution in curve-fitting deconvolution of OSL decay curves and (2) the relatively poor dating precision when using experimental fast component extraction. Here, a simple mathematic solution for fast component extraction is presented that is not relying on curve-fitting deconvolution and can easily be adopted into routine dating practices. By using specifically selected data points from smoothed OSL decay curves, the precision of equivalent doses calculated using the extracted fast component can be improved over equivalent doses calculated using bulk OSL. The fast component extraction is tested on a group of age-constrained samples containing both insufficiently bleached and sufficiently bleached deposits. Fast component OSL ages are as accurate as bulk OSL ages for the sufficiently bleached deposits, but more accurate for samples where bulk OSL is affected by insufficient bleaching. We also demonstrate how using a curve smoothing procedure can improve dating precision in case of both sufficiently and insufficiently bleached deposits.     

Annual dose assessment for luminescence and ESR dating: evaluation of nuclides mobility

The mobility of nuclides depends on their distribution within different sediment phases. Using a soil science approach, three main phases can be distinguished, which, according to increasing stability, are:

— The mobile phase, which includes elements in aqueous solution or elements weakly bonded at the surface of minerals.

— The phase that can be mobilised, in oxides, amorphous or weakly crystallised minerals. It can possibly move.

— The resistant phase, which cannot move.

The proportion of nuclides in the different phases, analysed together with other paedological data, can give information on the local stability of the radioactivity and possibly allow evaluation of error limits and corrections that should be applied to the present dose rate for dating purpose. In the worst cases this can lead to the conclusion that dating would not be reliable. Two case studies show the potential of the approach, which still remains more qualitative than quantitative. In an archaeological site (Ladoux, Puy de Dôme, France), streaming surface water brings radioactivity characterised by radium in excess. In volcanic tephra (La Vestide, Bas Vivarrais, France), nuclide mobility is found to be negligible; therefore observed disequilibrium in the U series pre-existed the eruption.     

A new mathematical approximation of sunlight attenuation in rocks for surface luminescence dating

The attenuation of sunlight through different rock surfaces and the thermoluminescence (TL) or Optical stimulated luminescence (OSL) residuals clock resetting derived from sunlight induced eviction of electrons from electron traps, is a prerequisite criterion for potential dating. The modeling of change of residual luminescence as a function of two variables, the solar radiation path length (or depth) and exposure time offers further insight into the dating concept. The double exponential function modeling based on the Lambert-Beer law, valid under certain assumptions, constructed by a quasi-manual equation fails to offer a general and statistically sound expression of the best fit for most rock types. A cumulative log-normal distribution fitting provides a most satisfactory mathematical approximation for marbles, marble schists and granites, where absorption coefficient and residual luminescence parameters are defined per each type of rock or marble quarry. The new model is applied on available data and age determination tests.