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.     

Luminescence dating of young coastal deposits from New Zealand using feldspar

A new measurement protocol has been tested on K-feldspars from Whanganui Inlet and Parengarenga Harbour, New Zealand. A Single Aliquot Regenerative (SAR) dose protocol, using two successive infrared (IR) stimulations (post-IR IR SAR protocol) is setup for these young (<1000 years) coastal sediments. Significant anomalous fading (g _2days =7 %/decade) is observed using the conventional IR signal measured at 50°C. In contrast, the fading rate of the IR signal measured at elevated temperature (150°C) after the IR stimulation at 50°C (a post-IR IR signal) is not significant (g _2days ≤ 1 %/decade). Surprisingly low residual infrared stimulated luminescence (IRSL) signals were observed for a surface sample, suggesting that accurate ages as young as ∼50 years can be obtained for these recent deposits. IRSL ages ranging between 48±6 years and 1050±50 years are obtained from six samples, indicating that sediment accumulation has occurred at the two sites during the last millennia, despite a falling trend in relative sea-level in Whanganui Inlet and a stable relative sea-level at Parengarenga Harbour.     

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.     

IRSL and post-IR IRSL residual doses recorded in modern dust samples from the Chinese Loess Plateau

Using a set of modern/young (0 to about 200 years old) dust samples collected from the Chinese Loess Plateau the bleachability of IRSL measured at 50°C (IR₅₀) and post-IR₅₀ elevated temperature IRSL (measured at 225°C and at 290°C) is investigated by measuring the apparent (residual) doses recorded by these signals. Doses recorded by quartz OSL are used as a reference. Allowing for differences in dose rates it seems that both IRSL and post-IR IRSL signals yield residual doses that are significantly larger than the doses measured in quartz. These residual doses can be largely explained by thermal transfer caused by preheating. Nevertheless, we advise against the use of a low temperature preheat (<200°C) with IR₅₀ to date loess samples because, as has been reported before, the signal appears to be thermally unstable. In general, we conclude that it may not be advisable to apply post-IR IRSL dating to Chinese loess samples where residuals of up to ∼20 Gy are a significant fraction of the total dose. However, these residuals quickly become unimportant when dating older samples, and this is the age range in which post-IR IRSL dating is likely to be most useful.     

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.     

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.     

On the applicability of post-IR IRSL dating to Japanese loess

Recent work on infrared stimulated luminescence (IRSL) dating has focussed on finding and testing signals which show less or negligible fading. IRSL signals measured at elevated temperature following IR stimulation at 50°C (post-IR IRSL) have been shown to be much more stable than the low temperature IRSL signal and seem to have considerable potential for dating. For Early Pleistocene samples of both European and Chinese loess natural post-IR IRSL signals lying in the saturation region of the laboratory dose response curve have been observed; this suggests that there is no significant fading in nature. As a contribution to the further testing of post-IR IRSL dating, we have used 18 samples from two Japanese loess profiles for which quartz OSL and tephra ages up to 600 ka provide age control. After a preheat of 320°C (60 s), the polymineral fine grains (4–11 μm) were bleached with IR at 50°C (200 s) and the IRSL was subsequently measured at 290°C for 200 s. In general, the fading uncorrected post-IR IRSL ages agree with both the quartz OSL and the tephra ages. We conclude that the post-IR IRSL signal from these samples does not fade significantly and allows precise and accurate age determinations on these sediments.     

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.     

Changes in natural OSL sensitivity during single aliquot regeneration procedure and their implications for equivalent dose determination

Measurement of low temperature (90°C–120°C) Thermoluminescence (TL) sensitivity of natural quartz samples subjected to pre-heating and optical stimulation indicate that significant sensitivity changes can occur during measurement of the natural Optically Stimulated Luminescence (OSL). During the measurement of natural signal, the luminescence sensitivity of samples can change by 40%. The sensitivity changes both during the initial preheat and the measurement of natural OSL. The currently used version of Single Aliquot Regeneration (SAR) protocol measures and corrects for the sensitivity changes after preheat and readout of natural OSL. However, it does not take into account the changes in sensitivity during the readout of the natural signal. We therefore developed a correction procedure so that both the natural and the regenerated OSL intensities can be measured and plotted with the same sensitivity and suggest that in the absence of such a correction, a considerable fraction of the SAR based ages could have systematic errors. The correction for the sensitivity is based on the use of sensitivity of 110°C TL quartz peak, which is correlated to OSL signal (Murray and Roberts, 1998). The use of 110°C peak provides a reasonable measure of the changes in OSL sensitivity of quartz. A modified Natural Sensitivity Corrected-SAR (NSC-SAR) procedure, that comprises the measurement of, 1) the TL intensity of 110°C peak for a test dose on sample as received (i.e. natural sample) and, 2) the sensitivity of the 110°C peak of the same sample after the preheat and read out of the natural OSL, is proposed. This ratio, termed as Natural Correction Factor (NCF), then provides a way to correct for sensitivity changes. Results on samples from diverse depositional environments indicated that the NSC-SAR consistently (without exception) provided improved distribution in paleodoses i.e. a lower scatter compared to the standard SAR protocol. In addition, the use of this protocol also resolved anomalous cases where the intensity of natural OSL was significantly above the saturation intensity of the regenerated OSL. Implicitly, this study implies a caution on the use of palaeodoses obtained from single grains as such a correction is not possible in the currently used automated single grain OSL measurement systems. The only way now on will be to analyze aliquots with only a grain on them.     

Comparing different post-IR IRSL approaches for the dating of Holocene coastal foredunes from Ruhnu Island,Estonia

Different post-IR Infrared Stimulated Luminescence (IRSL) approaches are applied to sediments from a Holocene coastal foredune sequence on Ruhnu Island in the eastern Baltic Sea. The comparison of D _e-values and ages determined by the different approaches is complimented by fading and bleaching experiments. The fading experiments imply strong fading of IRSL (50°C) signals and no fading of any of the post-IR IRSL signals, but this is not confirmed by the determined D _e-values. In fact, post-IR IRSL (150°C) D _e-values agree within errors with those calculated for IRSL (50°C). From the bleaching experiments it is inferred that the higher values observed for post-IR IRSL at more elevated stimulation temperatures (225°C/290°C) are likely related to either thermal transfer and/or slow-to-bleach components within the signal. For the dating of the Holocene foredune sequence of Ruhnu Island, the post-IR IRSL (150°C) approach is preferred and these agree with the limited independent age control available from radiocarbon dating. Accordingly, the sequence formed between ca. 7.0 ka and 2.5 ka ago.     

Transport and photochemical effects seen in stratospheric NO2 amounts

Column contents amounts of NO₂ were measured from our sites at 45°S, 53°S and 78°S using long path differential absorption spectroscopy. In spring, the two mid-latitude sites exhibit essentially the same smooth winter to summer transition. While this trend is also present in the Antarctic data, large amplitude oscillations with a period of approximately 9 days are superimposed on this trend. These oscillations are explained in terms of transport of mid-stratospheric air from more poleward or more equatorial latitudes.The observed night-time decay of NO₂ is shown to agree with a simple N₂O₅ chemical conversion scheme.     

Co-ordinated EISCAT-MICADO interferometer measurements of neutral winds and temperatures in E- and F-regions

The MICADO instrument has been built to measure temperature and wind in the E- and F-regions. It employs a thermally stable field-compensated Michelson interferometer to allow wind measurements. During the winter of 1988–1989, the MICADO instrument was operated at Sodankylä (67°22′N, Finland). Measurements were made by observing the O¹S (low thermosphere) and the O₁D lines (high thermosphere) emission. Two co-ordinated campaigns were organized with the EISCAT radar, which operated in special modes. Neutral wind and temperature are derived from EISCAT data. Results of the two instruments are shown. The differences between the two sets of results are discussed and show that most of the discrepancy is due to the presence of vertical winds during the observations where the magnetic activity was high.     

Low‐temperature catalytic CO2 hydrogenation with geological quantities of ruthenium: a possible abiotic CH4 source in chromitite‐rich serpentinized rocks

Metal‐catalysed CO₂ hydrogenation is considered a source of methane in serpentinized (hydrated) igneous rocks and a fundamental abiotic process germane to the origin of life. Iron, nickel, chromium and cobalt are the catalysts typically employed in hydrothermal simulation experiments to obtain methane at temperatures >200°C. However, land‐based present‐day serpentinization and abiotic gas apparently develop below 100°C, down to approximately 40–50°C. Here, we document considerable methane production in thirteen CO₂ hydrogenation experiments performed in a closed dry system, from 20 to 90°C and atmospheric pressure, over 0.9–122 days, using concentrations of non‐pretreated ruthenium equivalent to those occurring in chromitites in ophiolites or igneous complexes (from 0.4 to 76 mg of Ru, equivalent to the amount occurring approximately in 0.4–760 kg of chromitite). Methane production increased with time and temperature, reaching approximately 87 mg CH₄ per gram of Ru after 30 days (2.9 mgCH₄/g_ru/day) at 90°C. At room temperature, CH₄ production rate was approximately three orders of magnitude lower (0.003 mgCH₄/g_ru/day). We report the first stable carbon and hydrogen isotope ratios of abiotic CH₄ generated below 100°C. Using initial δ¹³C_CO2 of ‐40‰, we obtained room temperature δ¹³C_CH4 values as ¹³C depleted as ?142‰. With time and temperature, the C‐isotope separation between CO₂ and CH₄ decreased significantly and the final δ¹³C_CH4 values approached that of initial δ¹³C_CO2. The presence of minor amounts of C₂‐C₆ hydrocarbons is consistent with observations in natural settings. Comparative experiments at the same temperatures with iron and nichel catalysts did not generate CH₄. Ru‐enriched chromitites could potentially generate methane at low temperatures on Earth and on other planets.     

Rocket measurements of the equatorial airglow: MULTIFOT 92 database

The MULTIFOT airglow photometer payload was launched from Alcântara (2.5°S, 44.4°W) on a SONDA III rocket at 23:52 hrs local time on 31 May 1992. A total of ten photometers, six forward-looking and four side-looking, measured the height profiles of the airglow emissions O₂ Herzberg band system, 01557.7 run, NaD 589.3 nm, 01630.0 nm, OH(8,3) band R branch at 724.0 nm, O₂ Atmospheric (0,0) band at 762.0 nm and the sky background at 578 nm and 710 nm. At the time of launch, a ground-based airglow photometer observed the intensity variations of these emissions, together with the rotational temperature of the OH(9,4) band, and a sodium lidar measured atomic sodium concentration from 80 to 110 km.     

Luminescence characteristics and dose distributions for quartz and feldspar grains from Mumba rockshelter,Tanzania

Mumba rockshelter is a key archaeological site for the Middle and Later Stone Age occupation of East Africa, but its chronology has remained unresolved. We report the results of a dating study, focussing on the characterisation of the optically stimulated luminescence (OSL) and infrared stimulated luminescence (IRSL) properties of quartz- and potassium-rich feldspar grains. Quartz has previously proven troublesome for dating in East Africa. We identified five general types of quartz grain behaviour, based on the shapes of their OSL decay and dose–response curves. Dose recovery experiments and measurement of the natural samples revealed particular problems with quartz grains that had hyperbolic dose–response curves, low characteristic saturation doses and anomalously large changes in sensitivity between regenerative-dose cycles. The use of pulsed irradiation during measurement and standard and additional quality-assurance criteria during data analysis reduced the number of grains that suffered from these problems. We applied these procedures to individual grains of quartz from eight samples and, using appropriate statistical models, identified post-depositional mixing in three samples. The remaining samples had scattered equivalent-dose distributions typical of quartz grains that had received variable beta dose rates during burial. Stratigraphically consistent OSL ages were obtained for all but the deepest sample. Feldspar ages were estimated for the latter sample and three other samples, using the elevated temperature IRSL signal that exhibited low rates of anomalous fading. Fading-corrected feldspar ages for the latter three samples are consistent with their single-grain quartz ages, but single-grain dating is needed to address problems of post-depositional mixing.     

Petroleum infiltration of high-grade basement, South Norway: Pressure-Temperature-time-composition (P–T–t–X) constraints

Fluid inclusion data provide pressure–temperature–time–composition (P–T–t–X) constraints for an episode of petroleum infiltration of the crystalline basement in South Norway. Petroleum inclusions associated with pyrobitumen occur in postmetamorphic quartz veins in the Modum Complex. Three groups of fluid compositions have been shown, ranging from CH₄ ± CO₂ to condensates with alkanes up to C₁₅. The range in fluid composition is a result of petroleum decomposition at high temperature. Globular and massive pyrobitumen occurs in the quartz veins or in associated vein systems. Reflectance (%Rm) measurements of 3.20–3.35 correspond to a maximum temperature of 207–214°C for the pyrobitumen associated with group II and III inclusions. Geothermometry of chlorites included in the quartz show results of 226–231°C. Pressure conditions of trapping for all three groups of inclusion fluids have been estimated to 520–985 bar at 220°C. The pressure range is probably a result of fluctuations caused by repeated fracture opening and sealing due to seismic activity coupled with mineral growth. A lack of systematic textural relationships between the three groups of inclusions and similar pressure–temperature estimates for all fluid types indicate trapping at similar times and a process of rapid change. Fluid migration in fractures from an overlying, overpressured sedimentary basin into a dry, crystalline basement best explains the observed P–T–t–X constraints.     

Technological aspects of Mesopotamian Uruk pottery: estimating firing temperatures using mineralogical methods,thermal analysis and luminescence techniques

The Middle Uruk phase in Mesopotamia (3600–3500 bc) has been characterised by the massive production of “bevelled rim bowls” (BRBs). They are characterised by their similar shape and volume in Mesopotamia and surroundings. However, their production method has not been studied in detail, including the firing temperature. The determination of the firing temperature of ancient pottery has been attempted by studying mineral phase transformation sequences; although, very little knowledge exists about such transformations in mixtures or thermal analyses. These methods usually provide imprecise firing temperatures between 500 and 800 °C, as other factors such as the raw materials or firing time and conditions must be considered. As an alternative, luminescence techniques have been tested with promising results, as they have provided reliable maximum firing temperatures for ancient pottery at mild conditions (below 600 °C) with high precision. In this work, the firing temperatures of BRB samples from two archaeological sites located in the Middle Euphrates Valley (Syria) have been studied using mineralogical, chemical and thermal analysis. Both mineral characterization techniques and thermal analyses show agreement and firing probably below 600–700 °C. Luminescence yields ambiguous results but circumstantial evidence on the firing temperature between 400 and 550 °C.     

Review and assessment of the potential of post-IR IRSL dating methods to circumvent the problem of anomalous fading in feldspar luminescence

Quartz has been the main mineral used for optically stimulated luminescence (OSL) dating of sediments over the last decade. The quartz OSL signal, however, has been shown to saturate at relatively low doses of ～200–400 Gy, making it difficult to be used for dating beyond about 200 thou-sand years (ka), unless the environmental dose rate is low. The infrared stimulated luminescence (IRSL) from feldspars has been shown to continue to grow to higher dose levels than quartz OSL. The application of IRSL dating of feldspars, however, has long been hampered by the anomalous fading effect. Recent progress in understanding anomalous fading of the infrared stimulated luminescence (IRSL) signals in potassium-feldspar has led to the development of post-IR IRSL (pIRIR) protocols and also a multiple elevated temperature (MET) stimulation (MET-pIRIR) protocol. These procedures have raised the prospect of isolating a non-fading IRSL component for dating Quaternary deposits containing feldspars. In this study, we review the recent progress made on (1) overcoming anomalous fading of feldspar, and (2) the development of pIRIR dating techniques for feldspar. The potential and problems associated with these methods are discussed.     

Degradation of Archaeological Wood Under Freezing and Thawing Conditions—Effects of Permafrost and Climate Change

The degradation of archaeological wood at freezing and thawing temperatures is studied at the site of Qajaa in West Greenland through a combination of environmental monitoring, measurement of oxygen consumption and microscopy of wood samples. Permanently frozen wood is still very well preserved after 2–4000 years, while wood samples that thaw every summer show attack by soft rot and an average density loss of 0.1 g cm^–3 (corresponding to 25% of the dry mass) over the past 27 years. Future increases in temperature may increase the decay rate significantly (Q₁₀ = 4.2 at 0–10°C) but the effects on site depend on local hydrology.     

Gravity waves from O2 nightglow during the AIDA '89 campaign III: effects of gravity wave saturation

The O₂ atmospheric (0–1) night airglow emitted within the gravity wave saturation region at ∼90–100 km can serve as a means of studying the wave activity. In this analysis, the atmospheric motions were described by a mean spectral model and an algorithm was developed to infer the wave kinetic energy density and momentum flux from variations in O₂ (0–1) airglow emission rate and rotational temperature. The method was applied to eight nights of data collected by MORTI, a mesopause oxygen rotational temperature imager, during the AIDA campaign of 1989 in Puerto Rico (18°N, 67°W). The observed r.m.s. fractional fluctuations of airglow emission rate and rotational temperature were of the order of ∼0.07–0.15 and ∼0.02–0.04, respectively, and the characteristic vertical wavelengths were estimated at ∼10 2 -20 km. The inferred r.m.s. horizontal velocities and velocity variances were found to be ∼12–25 m/s and ∼150–600 m²/s², with the majority of the horizontal velocity and its variance associated with low-frequency, large-scale wave motions. The estimated momentum fluxes, mainly contributed by high-frequency, small-scale waves, were ∼2–10 m²/s². These results are in good agreement with those obtained from other measurements using different observational methods at low and mid-latitudes.