OPTICAL DATING OF SINGLE AND MULTIPLE GRAINS OF QUARTZ FROM JINMIUM ROCK SHELTER,NORTHERN AUSTRALIA: PART I,EXPERIMENTAL DESIGN AND STATISTICAL MODELS*

Jinmium rock shelter is famous for the claims made by Fullagar et al. (1996) for the early human colonization and ancient rock art of northern Australia. These claims were based on thermo-luminescence ages obtained for the artefact-bearing quartz sediments that form the floor deposit at the site. In this paper, we outline the background to the optical dating programme at Jinmium, and describe the experimental design and statistical methods used to obtain optical ages from single grains of quartz sand. The results, interpretations, and implications of this dating programme are reported in a companion paper (Roberts et al. 7999, this volume).     

OPTICAL DATING OF ANTHROPOGENIC SEDIMENTS AT THE ARCHAEOLOGICAL SITE OF HERRENBRUNNENBUCKEL,BRETTEN-BAUERBACH (GERMANY)*

Optical dating was applied to natural and anthropogenic silts at an Iron Age settlement in southern Germany. The natural sediments were dated accurately and allowed study of the human impact on the landscape. The studied anthropogenic sediments were infills of cellars and ditches. Again, deposits derived from soil erosion proved to be datable using infrared-optically stimulated luminescence. However, optical dating of fine grained sediments was at its limits when sediments consisted of a mixture of bleached and unbleached grains. This is shown on sediments of known age originating from cellar infills. Improvements were obtained when using the 560 nm emission and a partial bleach approach. Experimental evidence shows that the D_E versus shine-time plot discloses insufficient bleaching only in cases in which all grains are insufficiently bleached to the same degree.     

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.     

Optical dating of alluvial deposits at the orogenic front of the andean precordillera (Mendoza,Argentina)

Well constrained numerical ages of alluvial fan sediments are key to understanding the chronology of alluvial episodes and tectonic activity at the front of the Andean Precordillera. We tested the application of radiocarbon and optically stimulated luminescence (OSL) dating in the distal part of an alluvial fan five kilometers north of Mendoza. For OSL dating a large number of aliquots (n > 70) — each composed of ∼50 quartz grains — were measured in order to obtain reliable burial ages despite scattered dose distributions. Owing to a feldspar contamination in all samples, an infrared stimulation was inserted before each OSL measurement, which reduced the feldspar OSL signal successfully. By using the minimum age model we obtained stratigraphically consistent burial ages of alluvial deposits in a depth profile. The uppermost ∼1 m of sediment is composed of debris flow deposits buried 770±76 years ago. Three plant remnants used for radiocarbon dating from the same layer, however, yielded ages younger than 350 years, which are interpreted to underestimate the depositional age. Underneath the debris flow, a major unconformity cuts a series of distal alluvial fan sediments with interstratified floodplain deposits, which are composed of sandy and calciterich silt layers, respectively. Three samples from this unit which were distributed over one meter of sediment thickness yielded statistically concordant OSL ages of 12.3±1.2 ka, 12.3±1.2 ka, and 11.7±1.1 ka. The deposition of these sediments during the latest Pleistocene coincides with a phase of cool and humid climate, which occurred before the alluvial fan propagated farther into the foreland. The overlying debris flow sediments are associated with alluvial fan incision during the arid Late Holocene.     

THE EFFECT OF HF ACID ETCHING ON THE MORPHOLOGY OF QUARTZ INCLUSIONS FOR THERMOLUMINESCENCE DATING

The assumption of isotropic etching in hydrofluoric acid of quartz grains prepared for thermoluminescence dating has been tested by optical and scanning electron microscopy. We have found that the rate of etch is very irregular over the surface of many grains and that some grains are attacked much more severely than others. The uncertainty introduced into TL dating by this effect is discussed.     

ONLY TIME WILL TELL: A REVIEW OF THE METHODOLOGY OF DIRECT ROCK ART DATING

Epistemology has not kept pace with the progress experienced in the direct dating of rock art. This paper reviews the experimental methods that have been developed in recent years. While many do provide important information about the possible age of rock art, it is of concern that the precipitate archaeological interpretations these data are used for are often not warranted. Some are attributable to not understanding the severe qualifications that apply to most dating results, others perhaps to over-enthusiasm on the part of some researchers. The introduction of archaeological dynamics into direct dating of rock art threatens the reliability of this young methodology. Some of the pitfalls are considered in this paper, and a general rationale for the direct dating of rock art is developed.     

DATING OF THE HOMINID (HOMO NEANDERTHALENSIS) REMAINS ACCUMULATION FROM EL SIDRÓN CAVE (PILOÑA,ASTURIAS, NORTH SPAIN): AN EXAMPLE OF A MULTI‐METHODOLOGICAL APPROACH TO THE DATING OF UPPER PLEISTOCENE SITES

The age of Neanderthal remains and associated sediments from El Sidrón cave has been obtained through different dating methods (¹⁴CAMS, U/TH, OSL, ESR and AAR) and samples (charcoal debris, bone, tooth dentine, stalagmitic flowstone, carbonate‐rich sediments, sedimentary quartz grains, tooth enamel and land snail shells). Detrital Th contamination rendered Th/U dating analyses of flowstone unreliable. Recent ¹⁴C contamination produced spurious age‐values from charcoal samples as well as from inadequately pretreated tooth samples. Most consistent ¹⁴C dates are grouped into two series: one between 35 and 40 ka and the other between 48 and 49 ka. Most ESR and AAR samples yielded concordant ages, ranging between 39 and 45 ka; OSL dating results permitted adequate bracketing of the sedimentary layer that contained the human remains. Our results emphasize the value of multi‐dating approaches for the establishment of reliable chronologies of human remains.     

PALAEOMAGNETIC AND MINERAL MAGNETIC STUDIES OF SEDIMENTS FROM PETRALONA CAVE,GREECE

Palaeomagnetic measurements on sediments from Petralona cave. Greece indicate a stable, single component remanence of normal polarity. Redeposition experiments established the ability of the sediments to acquire the direction of the geomagnetic field. Magnetic properties and Mössbauer spectra of sediments and magnetic concentrates show that magnetite, which is slightly non-stoichiometric, and haematite are present in the sediments from the cave. The magnetite dominates the magnetic properties and exhibits pseudosingle domain behaviour. Using rstimated deposition rates for the sediments in the cave. and the fact that U Th and ESR dates which can be stratigraphically correlated to the palaeomagnetic section range from 200 to 750 ka. implies that the section represents a time span of about 150 180 ka within the Brunhes epoch. From this. the age of a human cranium found in the cave 25 years ago is estimated to be not older than 620 ka.     

Optically stimulated luminescence dating of young fluvial deposits of the Middle Elbe River Flood Plains using different age models

In the last few decades optically stimulated luminescence (OSL) dating has become an important tool in geochronological studies. The great advantage of the method, i.e. dating the depositional age of sediments directly, can be impaired by incomplete bleaching of grains. This can result in a scattered distribution of equivalent doses (D_E), leading to incorrect estimation of the depositional age. Thoroughly tested protocols as well as good data analysis with adequate statistical methods are important to overcome this problem. In this study, samples from young fluvial sand and flood plain deposits from the Elbe River in northern Germany were investigated to compare its depositional ages from different age models with well-known historical dates. Coarse grain quartz (100–200 μm and 150–250 μm) and polymineral fine grains (4–11 μm) were dated using the single aliquot regenerative (SAR) dose protocol. The paleodose (D_P) was calculated from the DE data set using different approaches. Results were compared with the development of the Elbe River, which is well-documented by historical records and maps covering the last 1,000 years. Depending on the statistical approach it can be demonstrated that depositional ages significantly differ from the most likely depositional age. For the investigated coarse grain quartz samples all ages calculated from the MAM-3_UL, including their uncertainties, are within the historical documented age. Results of the polymineral fine grain samples are overestimating the historically documented depositional age, indicating undetectable incomplete bleaching. This study shows the importance of using an adequate statistical approach to calculate reliable OSL ages from fluvial sediments.     

CHARACTERIZING THE SEDIMENTARY HISTORY OF CAVE DEPOSITS,USING ARCHAEOMAGNETISM AND ROCK MAGNETISM,ATAPUERCA (NORTHERN SPAIN)

We use a combination of rock magnetism (anisotropy of magnetic susceptibility, AMS) and magnetic polarity to characterize cave deposits and as a proxy for sedimentary fabric. In three localities at the Atapuerca archaeological site (Galeria, Gran Dolina and Sala de los Cíclopes), magnetic foliation (K_max/K_int) is always greater than lineation (K_int/K_min), consistent with a primary, depositional, sedimentary fabric. Our results, although preliminary, reveal a higher degree of anisotropy in autochtonous deposits compared to allochthonous deposits, possibly indicative of a higher hydrodynamic regime in the former. At two localities the magnetic lineation (K_max) defines a cluster, which is thought to be antipodal to the palaeocurrent direction. Hence we are able to retrieve palaeoflow directions in deposits that otherwise lack any other sedimentary structure. We conclude that AMS is a powerful tool for determining the hydrodynamic character of depositional environments in cave sediments at the Atapuerca archaeological site. A better understanding of the depositional environment and how sedimentation occurred allows reconstruction of the karst evolution and ultimately a better definition of human interaction with the environment.     

THERMOLUMINESCENCE FROM UNIRRADIATED FLINTS: REGENERATION THERMOLUMINESCENCE

The ‘spurious’thermoluminescent glow from ground samples of flint is responsible for dating errors in the region of 10 000 years for grains less than 45 μm diameter or of 4000 years for larger grains. The glow is partly tribothermoluminescence and partly regeneration thermoluminescence and the conditions in which these arise or are accelerated have been found. It is shown that if thin polished slices are used rather than powder, the amount of such glow is negligible.     

Distribution in SAR palaeodoses due to spatial heterogeniety of natural beta dose

In luminescence dating of sediments, Mayya et al. (2006) pointed out that at single grain level, the beta dose for quartz grains is heterogeneous. This heterogeneity arises due the fact that the total potassium in sediment is contributed by few feldspar grains with up to 11–14% stoichiometric potassium (Huntley and Baril, 1997). Beta particles have a range of ∼2 mm, which is comparable to grain sizes and inter-grain distances. This fact implies that the spatial fluctuation of beta emitters (K-feldspars) around individual quartz grains results in heterogeneous dose deposition. These fluctuations therefore, lead to an inherent spread in palaeodoses received by individual quartz grains.     

LUMINESCENCE DATING OF SEDIMENTS—THE DETECTION OF HIGH EQUIVALENT DOSE GRAINS USING AN IMAGING PHOTON DETECTOR*

In this paper we describe quantitative measurements on the thermoluminescence of many single grains, made with an imaging photon detector. In several of the sediments examined a few bright grains were found which had a high equivalent dose (ED). Physical measurements made on these grains using binocular microscopy and analytical scanning microscopy enabled several possible explanations for the causes of the high ED grains to be rejected. Insufficient bleaching at deposition or the intrusion of grains from an older sediment were identified as the most probable explanation for these grains.     

Optically stimulated luminescence dating of heated materials using single-aliquot regenerative-dose procedure: a feasibility study using archaeological artefacts from India

Optically stimulated luminescence (OSL) dating of heated/fired materials of archaeological importance from various parts of India was attempted. A single-aliquot regenerative-dose (SAR) procedure was used for palaeodose determination in the quartz grains extracted from the heated materials using the luminescence produced by blue light stimulation. In most pottery samples, the palaeodose obtained using SAR-OSL is ∼6% lower than the palaeodose measured using thermoluminescence (TL) method. Broadly, there is good agreement between the SAR-OSL and TL ages of the artefacts and their archaeologically expected ages. The results suggest that routine dating of heated/fired materials using the SAR-OSL procedure is more practicable, especially when the TL sensitivity of the quartz grains is poor and availability of datable material is limited.     

THERMOLUMINESCENT AUTHENTICITY STUDY AND DATING OF RENAISSANCE TERRACOTTAS

A comparative study is made of the thermoluminescence (TL) of terracottas of the Renaissance era and some known limitations of such ware dating to the middle of the last century. The data shows that conclusions on authenticity of an unknown work can be reliably obtained using this scientific method. Also examples are presented of accurate dating of genuine terracottas despite a lack of knowledge about the environmental circumstances of each piece's archaeological past.     

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.     

THE AUTHENTICITY OF FIGURINES,ANIMALS AND POTTERY FACSIMILES OF BRONZES IN THE HUI HSIEN STYLE

For some 15 years the authenticity of a group of small pottery pieces, claimed to have originated in the Hui Hsien area of China, has been the subject of academic discussion and some dissension. The thermolumines-cent dating of 22 such pieces from 4 independent collections is reported following a review of archaeological evidence for the origin of the material and of scientific investigations that have previously been made in investigation of its authenticity. It is concluded that all the pieces are of modern origin and not some 2300 years old as their stylistic forms might suggest.     

INFRARED STIMULATED LUMINESCENCE DATING OF ARCHAEOSEDIMENTS

In this study the feasibility of infrared stimulated luminescence (IRSL) for dating loessic colluvial sediments, deposited as a result of human activity, is investigated. It is demonstrated that the ‘IRSL-clock’is reset after a few minutes of daylight exposure even under foggy weather conditions. Samples of independently known age were taken at the Neolithic Bruchsal Aue site in south-west Germany. Different laboratory procedures are tried and a method is suggested (narrow wave-length band in the blue, preheat at 220° C for 5 min) to overcome age underestimates. This laboratory technique yielded archaeologically reasonable ages for colluvial sediments and hollow fillings. The IRSL-ages demonstrate that the deposition of the colluvia is related to soil erosion triggered by human activities, such as wood clearing and agriculture. The successful dating of archaeosediments has a great potential for applications in environmental archaeology as well as in geomorphology and in particular for the reconstruction of man-landscape interactions in central Europe.     

OSL dating using quartz fine grains extracted from loess in Upper Palaeolithic sites of Nihewan Basin, northern China

Although radiocarbon (¹⁴C) dating, uranium-series dating, and optically stimulated luminescence (OSL) dating have been conducted for Upper Palaeolithic sites in the Nihewan Basin, northern China, there is room for constructing a detailed chronological framework. In this study, loess sediments collected from two Upper Palaeolithic sites, Youfang site and Hutouliang site, were dated using the single-aliquot regenerative-dose (SAR) OSL protocol. OSL measurements for palaeodoses estimation used fine-grained quartz samples extracted from loess. OSL dating results were obtained as 10–17 ka. These OSL ages were consistent with the related stratigraphy of Palaeolithic sites, archaeological evidence and independent ¹⁴C ages.     

Investigating the resetting of OSL signals in rock surfaces

There are many examples of buried rock surfaces whose age is of interest to geologists and archaeologists. Luminescence dating is a potential method which can be applied to dating such surfaces; as part of a research project which aims to develop such an approach, the degree of resetting of OSL signals in grains and slices from five different cobbles/boulders collected from a modern beach is investigated. All the rock surfaces are presumed to have been exposed to daylight for a prolonged period of time (weeks to years). Feldspar was identified as the preferred dosimeter because quartz extracts were insensitive. Dose recovery tests using solar simulator and IR diodes on both K-feldspar grains and solid slices taken from the inner parts of the rocks are discussed. Preheat plateau results using surface grains and slices show that significant thermal transfer in naturally bleached samples can be avoided by keeping preheat temperatures low. Equivalent doses from surface K-feldspar grains were highly scattered and much larger than expected (0.02 Gy to >100 Gy), while solid surface slices gave more reproducible small doses (mean = 0.17±0.02 Gy, n = 32). Neither crushing nor partial bleaching were found to be responsible for the large scattered doses from grains, nor did the inevitable contribution from Na-feldspar to the signal from solid slices explain the improved reproducibility in the slices. By modelling the increase of luminescence signal with distance into the rock surface, attenuation factors were derived for two samples. These indicate that, for instance, bleaching at a depth of 2 mm into these samples occurs at about ∼28% of the rate at the surface. We conclude that it should be possible to derive meaningful burial doses of >1 Gy from such cobbles; younger samples would probably require a correction for incomplete bleaching.