On the intrinsic accuracy and precision of luminescence dating techniques for fired ceramics

Luminescence dating techniques have been used extensively for archaeological and geological samples. Such techniques are based on thermally or optically stimulated signals. This paper presents simulations of several luminescence techniques for equivalent dose (ED) estimation for ceramic materials containing quartz. The simulations are carried out using a recently published comprehensive kinetic model for quartz, consisting of 11 electron and hole traps and centers. The complete sequence of the experimental protocols for several thermoluminescence (TL) and optically stimulated luminescence (OSL) techniques are simulated using the same set of kinetic parameters. The specific simulated protocols are: additive dose TL protocol, predose technique (both additive and multiple activation versions), phototransfer protocol, single aliquot regenerative optically stimulated luminescence (SAR-OSL) protocol, and SAR thermoluminescence protocol (SAR-TL). One hundred random variants of the natural samples were generated by keeping the transition probabilities between energy levels fixed, while allowing simultaneous random variations of the concentrations of the 11 energy levels. The relative intrinsic accuracy and precision of the protocols are simulated by calculating the equivalent dose (ED) within the model, for a given natural burial dose of the sample. The intrinsic accuracy of these techniques is estimated by simulating natural irradiation of the samples with a known burial dose, followed by simulation of the luminescence method used to recover the estimated dose ED. The percent difference between the burial dose and the ED value represents the simulated accuracy of the luminescence technique. The relative intrinsic precision of these techniques is estimated by fitting Gaussian probability functions to the ED values obtained with the 100 model variants. It is found that the various techniques can reproduce natural paleodoses in the range 10 mGy–10 Gy with a typical intrinsic accuracy of +1 to 10%. Techniques based on single aliquot protocols were found in general to be more precise than techniques requiring the use of multiple aliquots. In addition, techniques based on interpolation of experimental data were found to be consistently both more precise and accurate than those based on extrapolation of experimental data.     

The D e (T,t) plot: A straightforward self-diagnose tool for post-IR IRSL dating procedures

This study presents a new self-diagnose method for the recently developed post-IR infrared stimulated luminescence (pIRIR) dating protocols. This criterion studies the dependence of equivalent dose (D _e) on measurement-temperature (T) and time (t), by applying the D _e (t) analysis to the IRLS and pIRIR signals measured under different temperatures, and combines these D _e (t) plots into one, so-called the D _e (T, t) plot. The pattern of the D _e (T, t) plot is shown to be affected by anomalous fading, partial bleaching and non-bleachable signal. A D _e plateau can be achieved in the D _e (T, t) plot only when the effects of these factors are insignificant. Therefore, this plot can be used as a self-diagnose tool for the validity of pIRIR results. The D _e (T, t) analysis has been applied to four recently developed pIRIR protocols, using aeolian samples with different ages. The results show that this self-diagnose tool can be applied to different pIRIR protocols for validating the pIRIR dating results and evaluating the pIRIR measurement conditions.     

Roman traces in Germania magna: New thermoluminescence and pIRIR290 data from a lime kiln at Bergisch Gladbach,Germany

The applicability of a post‐infrared infrared stimulated luminescence (pIRIR₂₉₀) protocol and two different thermoluminescence (TL) protocols—a single aliquot regeneration (SAR) and a multiple aliquot additive dose (MAAD)—was tested on six polymineral fine‐grain (4–11 μm) samples extracted from the wall remains of a Roman lime kiln and a Roman roof tile. These remains had been excavated close to Bergisch Gladbach, which was at that time part of Germania magna. For the pIRIR₂₉₀ measurements, no dependence of D_e on first‐stimulation temperature was detectable, and the standard first stimulation temperature at 50°C was adopted. Fading tests and dose‐recovery tests were made for all samples. Background subtracted glow curves were recorded up to 480°C for TL after a preheat of 220°C for 120 s. A‐values were determined for all TL and pIRIR measurements. The results for all three protocols were fairly consistent, and TL and pIRIR₂₉₀ protocols are shown to be suitable to estimate reliable equivalent doses for the fired kiln walls. The resulting ages are in agreement with the expected time range—Roman Iron Age—and with independent age control provided by radiocarbon ages of animal bones and charcoal from the firing chamber.     

Stability of IRSL signals from sedimentary K-feldspar samples

Recent work has identified IR stimulated luminescence signals at elevated temperature from both potassium- and sodium-rich feldspars that have much lower anomalous fading rates than the conventional signal measured using IR stimulation at 50°C. This paper examines the stability of these signals for potassium-rich sedimentary feldspars. We show that the natural post-IR IRSL (pIRIR) signal from a 3.6 Ma old sample is in apparent saturation on a laboratory generated dose response curve, i.e. it does not show detectable fading in nature although a low fading rate is observed on laboratory time scales. We show that the pIRIR signal has a greater thermal stability than the IRSL signal and that the trend in increasing thermal stability is mirrored by a decreasing fading rate. We also investigate the effect of preheat temperature and IR stimulation power on the decay shape and conclude that the data can be explained in terms of either a single- or multiple-trap model. We present evidence that may suggest that at least part of pIRIR signal is derived from a high temperature trap (∼550°C thermoluminescence (TL) peak), although again the data can also be explained in terms of a single-trap model. Finally, we present dose response curves and characteristic curvature constants (D₀) values for various IRSL signals and conclude that the more stable signals saturate more quickly than the less stable signals and that the initial and final signals saturate at approximately the same level.     

The Firing Temperature of Pottery from Ancient Mesopotamia,Turkey, Using Luminescence Methods: A Case Study for Different Grain‐Size Fractions

The assessment of the firing temperature of a prehistoric pottery sample collected from ancient Mesopotamia, Turkey was studied using luminescence techniques. The methods for this estimation involved the observation of the thermal and pre‐dose sensitization with various re‐firing temperatures for both TL and the OSL signals. In the former case, the 110°C TL peak and the rest of the glow curve were used as proxies in this study. In the framework of a first attempt to investigate the impact of grain‐size dependence on the sensitization of the luminescence signals, the aforementioned study was performed with four different pottery grain‐size fractions: (i) less than 60 μm, (ii) 60–90 μm, (iii) 90–180 μm and (iv) 180–250 μm. The results clearly demonstrated the firing temperature mark of ～500°C in for the grain size of 90–180 μm, while—as in the case of the lower grain‐size fraction—a third proxy, the ratio of the pre‐dosed to the thermal sensitization, was seen to indicate the firing temperature. The remaining two grain‐size fractions failed to provide any meaningful results with regard to the firing temperature estimation. The dependence of the TL characteristics on the grain size was explained in the framework of the mixed mineralogy.     

Firing temperature of a clay core sample in a bronze tripod from Daxinzhuang Site in China using TL techniques

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.     

Thermospheric and mesospheric temperatures during geomagnetic storms at 23°S

Night-time thermospheric temperatures, T63o, and mesospheric rotational temperatures, T(OH) and T(O₂), have been measured at Cachoeira Paulista (23°S, 45°W, 16°S dip latitude), located in both the equatorial ionospheric anomaly and the South Atlantic Geomagnetic Anomaly, with a Fabry-Perot interferometer and a multi-channel tilting filter-type photometer, respectively. The thermospheric temperatures are obtained from the Doppler line broadening of the OI 630.0 nm emission and the mesospheric rotational temperatures from the OH(9,4) and O₂A(0,1) band emissions. Measurements made during three geomagnetic storms showed that the nocturnal mean values of T₆₃₀ during the recovery phase of the storms were lower than those observed during quiet time and from model predictions. Also, the nocturnal mean value of the T₆₃₀ soon after the SSC event on 27 June 1992 was higher than the quiet time and model predictions. The observed mesospheric nocturnal mean rotational temperatures, T(O₂) and T(O₂), were unaffected by the storms. A comparison of the night-time observed temperatures T₆₃₀, T(OH) and T(O₂) with those calculated using the MSIS-86 model is also presented.     

An improved OSL chronology for the Still Bay layers at Blombos Cave,South Africa: further tests of single-grain dating procedures and a re-evaluation of the timing of the Still Bay industry across southern Africa

This paper presents a series of new single-grain optically stimulated luminescence (OSL) ages for the Still Bay at Blombos Cave, South Africa, and compares them to previously published OSL, thermoluminescence (TL) and electron-spin resonance (ESR) ages for this site. Details are provided about the measurement and analytical procedures, including a discussion of the characteristics of the OSL signals of individual quartz grains. This forms the basis for further investigations into the sensitivity of the equivalent dose (D_e) estimates to a range of different analytical approaches, including changes in the size of the test dose, the choice of signal integration interval, the subtraction of an appropriate background, and isolation of the most light-sensitive (‘fast’) component of quartz OSL. We also report the results of an inter-operator test of D_e determination using seven new samples from Blombos Cave, and demonstrate the reproducibility of results obtained for two samples that had been dated previously at another laboratory and were measured and analysed again in this study. Together, these tests validate the robustness of the Blombos Cave single-grain OSL age estimates to a variety of alternative OSL dating procedures. We have incorporated, for the first time, these ages for Blombos Cave into a data set of all single-grain OSL ages for Still Bay and Howieson's Poort sites across southern Africa, and have used a statistical model to re-evaluate the timing and duration of the Still Bay industry. We calculate the most plausible start and end dates of the Still Bay as 72.2 ka and 71.3 ka, respectively – amounting to a duration of 0.9 ka – and estimate (with conventional 95% confidence) that this industry began no earlier than 75.5 ka, ended no later than 67.8 ka and lasted no longer than 6.6 ka.     

Temperature anisotropy of drifting ions in the auroral F-region,observed by EISCAT

During relative drifts between the ions and the neutrals perpendicular to the geomagnetic field, the ion temperature in the auroral F-region becomes anisotropic with a higher temperature perpendicular than parallel to the magnetic field (T_⊥ >T_∥). It has been shown that for a gyrotropic ion velocity distribution the ion temperatures T_⊥ and T_∥ can be expressed as a function of the neutral temperature and of the squared normalized relative ion-neutral drift, with parameters β_⊥ and β_∥ describing the anisotropy and the collision process.In this paper, five increases of the F-layer ion temperature and ion drift velocity, found in EISCAT-CP1F data, were analyzed to obtain information about the anisotropy and the collision process. In the CP1F experiment, the angles between the magnetic field line ending in Tromsø and the antenna directions remain small, and the ion drift velocities of the investigated events in general were below 1500 m/s. Thus the ion velocity distributions were approximated by a bi-Maxwellian, and NO⁺ was assumed to remain a minor constituent at the F-layer maximum. For a quantitative analysis, generalized theoretical β-values for a bi-Maxwellian ion velocity distribution drifting through a mixture of different neutral components and for arbitrary observation directions were calculated. With these expressions it was possible to compare the drift dependence of the measured ion temperature for every antenna position directly with the theory. A statistical analysis of the heating events showed a good correlation between the ion temperatures of Tromsø, Kiruna and Sodankylä and the squared normalized ion drift, and values β_T, β_K, β_S could be calculated by linear regression. The fitted curves corresponded well with theoretical curves for a bi-Maxwellian velocity distribution of O⁺ ions drifting through a neutral atmosphere consisting of O and N₂.     

Anomalous fading and crystalline structure: Studies on individual chondrules from the same parent body

Plagioclase feldspar is the major luminescent mineral in meteorites. Thermoluminescence (TL) characteristics, peak temperature (T_m), 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 T_m (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 T_m 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.     

Measurements of gradients in ionospheric parameters with a new nine-position experiment at Millstone Hill

A new nine-position experiment is now routinely carried out with the Millstone Hill incoherent scatter radars which allows estimation of spatial gradients in the measured ionospheric scalar parameters N_e, T_e, and T_i, and in the components of the ion velocity vector v_i. Use of this technique results in improved estimates of basic and derived parameters from incoherent scatter data at times of significant gradients. We detail the data analysis method and present the first results from this new experiment. The gradients in N_e and in the components of vi are used to compute the motion term in the ionospheric F region continuity equation ▿ · (Nv), which is then combined with ∂N/∂t to estimate the O⁺ recombination rate β at night. Meridional neutral winds U_mer are computed from the field-aligned ion velocity v_∥ and a calculation of the O⁺ diffusion velocity v_d, and it is found that horizontal gradients in the ion velocity field at times significantly affect the calculation of the neutral winds.     

Comparison of incoherent scatter observations of electron density,and electron and ion temperature at Millstone Hill with the International Reference Ionosphere

Millstone Hill incoherent scatter (IS) observations of electron density (N_e, electron temperature (T_e) and ion temperature (T_i) are compared with the International Reference Ionosphere (IRI-86) for both noon and midnight, for summer, equinox and winter, at both solar maximum (1979–1980) and solar minimum (1985–1986). The largest difference inN_e is found in the topside, where values of N_e given by IRI-86 are generally larger than those obtained from IS measurements, by a factor which increases with increasing height, and which has a mean value near two at 600 km. Apart from the bottom of the profile, which is tied to the CIRA neutral temperature, the IRI-86 T_e model has no solar cycle variation. However, the IS measurements during the summer reveal larger T_e at solar maximum than at solar minimum. At other seasons higher T_e at solar maximum occurs only during the daytime at the greater heights. Nighttime T_e is shown by the IS radar to be generally larger in winter than in summer, an effect not included in the IRI. This is apparently due to photoelectron heating during winter from the sunlit ionosphere conjugate to Millstone Hill. The day-night difference in T_i given by IRI-86 above 600km is not as large in the IS measurements.     

Performance tests using the Lexsyg luminescence reader

This study presents test measurements on a Lexsyg luminescence reader, acquired by the Giessen luminescence group. The reader is of the type Standard, hence designed for routine determination of palaeodoses using quartz or K-feldspars. The tests include measurements of the stimulation powers, preheat temperatures, OSL- and TL-curves, as well as dose recovery tests and calibration measurements using highly sensitised calibration quartz. A comparison of D _e values determined using a Lexsyg reader with single grain D _e-values, which have been previously obtained on a Risø reader, is also presented. The results imply that the Lexsyg reader is a highly reliable measurement device with high reproducibility, yielding instrumental uncertainties of around 0.3%.     

Electric fields and currents in the equatorial electrojet deduced from VHF radar observations—I. A method of estimating electric fields

Using the measured Doppler spectra of the VHF backscatter radar signals from type II ionization irregularities in the equatorial electrojet (EEJ) at Thumba (dip. 56′S), the height profiles of the phase velocity V_p of the plasma waves in the EEJ are determined. It is shown that the east-west electrostatic field E_y in the EEJ can be deduced from the experimental height profiles of V_p using an appropriate model of ion and electron collision frequencies. The theoretical basis and the practical application of the method for deducing E_y are described. The usefulness of the method even when type I irregularities are present at the higher altitudes of the EEJ is demonstrated.It is shown that the collision frequencies of ions and electrons are likely to have a significant diurnal variation, which may be caused by diurnal variations of the neutral densities and temperatures in the E-region.     

The impact of gravity waves on nitric oxide in the lower thermosphere

Observations of nitric oxide (NO) by the Solar Mesosphere Explorer (SME) during equinox indicate a lower-thermosphere equatorial minimum which is at variance with theoretical predictions. To address this discrepancy a zonally averaged model of the thermosphere and upper mesosphere is used to evaluate the influence of a latitude variation in turbulence. Five numerical simulations were performed with different latitude structures of eddy diffusion (K_T), ranging from uniform in latitude, peaks at low, mid-, or high-latitude, to a hemispherically asymmetric distribution. A local increase in eddy diffusion causes the lower thermosphere to cool and induces a latitude pressure gradient that drives horizontal and vertical winds. The circulation, turbulent transport and temperature dependent chemistry act to change the distribution of species. Comparison of the model predictions of NO with SME data, and simulated wind and temperature structure with empirical climatology, indicates a preference for a midlatitude peak in K_T.     

Computer simulations of the seasonal variations of the ionospheric equatorial anomaly in East Asia under solar minimum conditions

The previous dynamical, computer simulation model of the ionosphere at low latitudes of Chan H. F. and Walker G. O. (1984a, J. atmos. terr. Phys. 46, 1103; 1984b, J. atmos. terr. Phys. 46, 1113) has been modified to (1) include photoionization of molecular species NO⁺, N₂⁺ and O₂⁺ below 300km, (2) decouple the ionization and wind calculations below 180 km and (3) expand the geographical coverage to 46°N-30°S latitude. The first two modifications improved the model stability and the latter reduced the effect of the lateral boundaries on the equatorial anomaly. Results are presented for the representative seasonal months of January, April and July for East Asia, during solar minimum, comprising latitudinal-local standard time (120°E) contour plots of (1) the atmospheric pressure, (2) the computed meridional wind at 300 km, (3) the foF2 and (4) hmF2, together with latitudinal profiles of foF2 and N_T (electron content) showing the daytime development and nighttime decay of the equatorial anomaly.Comparisons have been made between the computer simulations and various experimental measurements of foF2, M(3000) F2 and N_T obtained in East Asia during periods of low solar activity. Most of the gross features of the development and decay of the equatorial anomaly at the various seasons were reproducible by the model simulations, the best agreement occurring for the equinoctial month of April.     

FIFTY YEARS OF LUMINESCENCE DATING*

Luminescence techniques for dating both heated materials (e.g., pottery and burnt stone) and sediments have gone through three phases in the past 50 years. The first 22 years, from 1957 to 1979, were devoted to thermoluminescence (TL) techniques applied to heated material. In the next six years, from 1979 to 1985, it was found that TL dating could be applied to sediments. However, the TL signals of both quartz and feldspar grains observed for modern sediments were small, but were not zero, thus making them useful only for older sediments. A new luminescence signal that was totally zeroed by exposure to sunlight for a relatively short period of time, a few hours or less, was found; this led to the development of optically stimulated luminescence (OSL) dating techniques in 1985. Further developments have continued to the present day. Within the past 22 years, 1999 was also a year with major developments. A reliable procedure for single aliquots of quartz that have a rapidly bleached (‘fast’) OSL component was formalized and an instrument that allowed rapid measurement of equivalent doses for single grains was constructed. These developments have led to OSL becoming a major dating tool in Quaternary geology, at least for the past 100 000 years, and in archaeology, particularly as related to the dispersal of modern humans.     

Polar thermospheric Joule heating,and redistribution of recombination energy in the upper mesosphere

Kellogg, W. W. (1961, J. Met. 18, 373) suggested that transport of atomic oxygen from the summer into the winter hemisphere and subsequent release of energy by three body recombination, O + O + N₂→O₂ + N₂ + E, may contribute significantly to the so-called mesopause temperature anomaly (increase in temperature from summer to winter). Earlier model calculations have shown that Kellogg's mechanism produces about a 10% increase in the temperature from summer to winter at 90 km. This process, however, is partly compensated by differential heating from absorption of UV radiation associated with dissociation of O₂. In the auroral region of the thermosphere, there is a steady (component of) energy dissipation by Joule heating (with a peak near 130 km) causing a redistribution and depletion of atomic oxygen due to wind-induced diffusion. With the removal of O. latent chemical energy normally released by three body recombination is also removed, and the result is that the temperature decreases by almost 2% near 90 km. Through dynamic feedback, this process reduces the depletion of atomic oxygen by about 25% and the temperature perturbation in the exosphere from 10% to 7% at polar latitudes. Under the influence of the internal dynamo interaction, the prevailing zonal circulation in the upper thermosphere (small in magnitude) changes direction when the redistribution of recombination energy is considered. The above described effects are very sensitive to the adopted rates of eddy diffusion. They are also strongly time dependent and are significantly reduced for disturbances associated with magnetic storms.     

Rock surface luminescence dating of prehistoric rock art from central Iberia

Rock art paintings are notoriously difficult to date numerically. Recently, luminescence dating has been shown to provide reliable rock surface burial ages in various archaeological settings. Here we use the cross-cutting relationship between a fallen rock and two paintings of the Iberian Levantine (older) and Schematic (younger) styles to constrain the age of the paintings by dating the rockfall event using rock surface luminescence dating. Infrared-stimulated luminescence (IRSL) signals as a function of depth into the buried face of the talus border indicate that the IRSL signal measured at 50°C (IR₅₀) was sufficiently reset to a depth of about 1.6 mm prior to burial. An uncorrected IR₅₀ age of 1.6 ± 0.2 ka was calculated for the rockfall event by dividing the surface equivalent dose (D_e) by the total dose rate. This age was corrected using both conventional and field-to-laboratory saturation approaches to yield indistinguishable ages of 2.7 ± 0.5 and 2.9 ± 0.3 ka, respectively. Since the panel with Schematic art was first available to the artist after the rockfall, we conclude the Schematic rock art at Villar del Humo is younger than ~2.9 ka. The Levantine rock art was painted on a panel constrained by the talus boulder before detachment, and so it is likely to be older than ~2.9 ka.     

The effect of rapid changes in ionospheric flow on velocity vectors deduced from radar beam-swinging experiments

The effects on the horizontal ionospheric velocity vectors deduced from radar beam-swinging experiments, which occur when changes in the flow take place on short time scales compared with the experiment cycle time, are analysed in detail. The further complications which arise in the interpretation of beam-swinging data, due to longitudinal gradients in the flow and to field-aligned flows, are also considered. It is concluded that these effects are unlikely to seriously compromise statistical determinations of the response time of the flow, e.g. to changes in the north-south component of the IMF, such as have been recently reported by Etemadi et al. (1988, Planet. Space Sci. 36, 471), using EISCAT ‘Polar’ data.