URANIUM‐SERIES AND LUMINESCENCE DATING OF VOLCANIC LITHIC ARTEFACTS*

U‐series dating was used to determine the growth rate of a feldspar‐to‐clay weathering rind in a mid‐Holocene Cascade–Olcott tradition andesite core, and luminescence dating (last exposure to sunlight) was used to date fine‐grained feldspars scraped from the surfaces of similar buried artefacts from a ¹⁴C‐sediment‐dated archaeological site (45KI464) on the wet western slope of the Cascade Mountains of Washington. For U‐series dating, we measured ²²⁶Ra excess (²²⁶Ra excess =²²⁶Ra –²³⁰Th) in five stratigraphic depth controlled rind scrapings. ²³⁸U, ²³²Th and ²³⁰Th were counted by alpha spectrometry, and ²²⁶Ra and ²¹⁰Pb were counted by gamma spectrometry on each sub‐sample.     

ESR Dating of Tooth Enamel: Comparison with AMSC at El Castillo Cave, Spain

At El Castillo, in Cantabrian Spain, uncalibrated AMS¹⁴C dating has shown the transition from Mousterian to Aurignacian to occur at 39·3±1·6 kaBP. We found ESR tooth enamel ages from the basal Aurignacian level at El Castillo to be 36·2±4·1 ka (early and linear uptake). The enamel and dentine had very low U contents, but ESR ages are strongly dependent upon knowledge of the moisture content history of the sediments. Although the Aurignacian ESR age is 8% younger than the weighted average uncalibrated AMS¹⁴C age of 39·6±1·3 ka obtained from charcoal samples, we have shown that the methods agree within experimental uncertainty. However, since no precise¹⁴C calibration yet exists for this period of time, we are unable to specify which of the ages is more accurate, nor are we able ascribe the apparent age discrepancy to a particular deficiency in the ESR method.     

ANOMALOUS CARBON-13 VALUES FOR FIBRE TEMPER IN CERAMICS*

Ceramic vessels from Later Stone Age sites in the Seacow river valley, South Africa, were heavily tempered with C4 grasses. However, most δ¹³C values of the temper fall between the known δ¹³C ranges for C4 and C3 grasses. Among possible C3 additives that could skew the signal, ground bone, animal dung, alpine grass, Karoo scrub ash, and humic acid contamination are eliminated. The sherd surfaces yield fatty chars with C3-like values. Although these are not enough to account for all the skewing, they represent only the final cooking event. They were preceded by many such events in which fat was absorbed into the C4 grass then charred to soot by later periods in the fire. Thus organic carbon with the isotope composition of the fat built up while the vessel remained in use.     

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.     

THE CHRONOSTRATIGRAPHY AND GEOARCHAEOLOGICAL SIGNIFICANCE OF AN ALLUVIAL GEOARCHIVE: COMPARATIVE OSL AND AMS 14C DATING FROM GREECE*

The Basin of Phlious in southern Greece is known for its thick colluvial and alluvial deposits from the Holocene. It offers a good opportunity to reconstruct the history of Holocene soil erosion and its interaction with historical farming activities. In this study, we present new results based on optically stimulated luminescence (OSL) dating from the Basin of Phlious. The comparison between OSL and ¹⁴C AMS ages shows good agreement, and demonstrates the need for the detection of insufficiently bleached OSL samples in order to obtain accurate results. The discovery of a Neolithic site, buried under thick alluvial deposits, confirms the hitherto postulated Neolithic human impact on the landscape.     

DETECTING FORGERIES AMONG ANCIENT GOLD OBJECTS USING THE U,Th–4He DATING METHOD*

Forgeries of ancient gold objects are prevalent in almost every collection and some public exhibitions in the past have been exposed as containing forgeries to an embarrassing extent. This situation comes from the fact that it is sometimes impossible to unequivocally recognize forgeries based on their patina or manufacturing and decoration characteristics. We demonstrate that for 13 ancient gold objects the time of their last melting process can be estimated using the U,Th–⁴He dating technique. The extremely small quantities of radiogenic ⁴He found, due to the young age and small sample size, require the use of a specially designed ultrasensitive mass spectrometer. We show that the proposed method is a powerful, and the only, quantitative tool in archaeometry for discriminating between fake and genuine ancient gold objects.     

BAYESIAN ANALYSIS OF PLEISTOCENE CHRONOMETRIC METHODS*

Bayesian analysis of radiocarbon dates on Holocene archaeological sites has become well established. Application to Pleistocene sites dated by multiple techniques would be advantageous. This paper develops the necessary mathematical apparatus in the form of likelihoods for luminescence dating, and uranium‐series dating, and considers the possibility for amino‐acid racemization dating. Application of the new methods is illustrated using the stratigraphic sequences of dates from the sites of Saint‐Césaire and La Chaise‐de‐Vouthon. For application to amino‐acid racemization dating, fuller publication of data is found to be required.     

A NEW DATING METHOD FOR HIGH‐CALCIUM ARCHAEOLOGICAL GLASSES BASED UPON SURFACE‐WATER DIFFUSION: PRELIMINARY CALIBRATIONS AND PROCEDURES*

The first European settlers came to North America in the early 17th century using glass in the form of containers and decorative objects. Thus, glass is a horizon marker for all historic period settlements and a potential source of chronometric dates at archaeological sites belonging to the historic period in the Americas. We have developed a new absolute dating method based upon water diffusion into the surface of manufactured glasses that predicts diffusion coefficients based upon variation in glass chemical constituents. Low‐temperature (< 190°C) hydration experiments have been performed on a set of five high‐calcium (21.7–28.3%) glasses that were used to manufacture wine bottles from the 17th?19th centuries. Infrared spectroscopy and secondary ion mass spectrometry was used to model the water diffusion/alkali exchange process. The ability of the model to accurately predict archaeological ages was evaluated with artefacts recovered from ceramic‐dated contexts at Thomas Jefferson's plantation known as Monticello.     

SIMS‐SS,A NEW OBSIDIAN HYDRATION DATING METHOD: ANALYSIS AND THEORETICAL PRINCIPLES*

The water diffusion mechanism in obsidian has been revisited with the advent of a new dating approach employing secondary ion mass spectrometry (SIMS). The water diffusion SIMS(+) profile and the concept of a surface saturation (SS) layer in obsidians both provide a sound basis for the new diffusion age equation (SIMS‐SS) and are supported by dated world examples ( Liritzis et al. 2004 ). Here, we present the basic physical–chemical analysis of the mass transport phenomenon on which the new dating method is based. The crucial age parameter of the SIMS‐SS dating approach for archaeological obsidians—that is, the surface saturation (SS) layer—is supported by both theoretical and experimental data.     

DIRECT GAMMA-RAY SPECTROMETRIC DATING OF FOSSIL BONES: PRELIMINARY RESULTS

A non-destructive gamma-ray spectrometry was used for direct dating of fossil animal and human bones taken from an alluvial Quaternary site in northern Italy. The ages were obtained using the U-Pa method: the chronological results are in agreement with palaeofaunal indicators and taphonomic data. The ages of two samples showed concordance with the U-Th method; in a third case good agreement was also found with the radiocarbon date, thus lending credence to our modified gamma spectrometric method.     

Chemical U-Th-Pb geochronology: A precise explicit approximation of the age equation and associated errors

In a single decaying system, the age determined from the exponential decay law is directly related to its linear Maclaurin approximation. This relationship can be additively extended to several decaying systems resulting in the same daughter element, by using proportionality functions, thus allowing an explicit formulation of the age as a function of element concentrations. The values of the binary proportionality function for the ²³⁸U-²³⁵U-Pb system and the ternary proportionality function for the ²³²Th-²³⁸U-²³⁵U-Pb system were determined by iterations of the exponential decay formula up to 4 Ga, with a step of 10 Ma, for a set of 24 different U/Th ratios. From the iteration data, the expressions of the two functions and the associated coefficients were determined by polynomial regression and mathematical programing on conveniently separated time and compositional intervals. Additional time- and composition-dependent age corrections optimized by mathematical programming of the residuals lead to an accuracy of 0.005 Ma of the resulting age. The error propagation can be traced through all the operations defined by explicit formulas according to simple error propagation rules, finally allowing the calculation of the standard error of the result. The formulas and parameters derived can be used in a calculation spreadsheet.     

ESR Dating of Micoquian Industry and Neanderthal Remains at K?lna Cave, Czech Republic

Electron spin resonance (ESR) and mass spectrometric U-series dating has been carried out on teeth recovered from K?lna cave during the excavations of 1961–76. Linear and early uptake (LU and EU) age estimates are similar due to low internal U content of the teeth. In general, ESR ages decrease upward in the section, but teeth from stone-rich (“lumpy”) layers give anomalously young ages, due to uneven dose-rate distribution. Elephant molars also give anomalously low ages, apparently due to self-absorption of gamma dose. Disregarding anomalous data, earliest appearance of Micoquian lithics and last occurrence ofDicerorhinus kirchbergensisin layer 9b is dated to 69±8 ka, which places them near the oxygen isotope stage (OIS) 5a/4 boundary. Neanderthal remains and the latest occurrence of Micoquian lithics in level 7a are dated to 50±5 ka, in good agreement with an uncalibrated radiocarbon date for this level of about 45 ka. The interstadial character of the fauna of this level also agrees with its date which places it in OIS 3. We also report that three stadial/interstadial cycles recognized in the lithological, faunal and palynological record of levels 9b through 7a at Kölna occurred during the timespan from about 70 to 50 ka.     

Geochronology of Palaeolithic cultures in the Hiran Valley, Saurashtra, India

The U and Th concentrations of 16 miliolite samples from the Hiran Valley in Saurashtra ranged from 0·3 to 2·14ppm and 0·12 to 0·82ppm respectively. The ²³⁴U/²³⁸U activity ratio ranged from 1·09 to 1·16, with a mean of 1·12±0·02. It agrees well with the seawater value of 1·14±0·02 within the quoted errors. Nine of the samples were datable by the ²³⁰Th/²³⁴U method and the ages ranged from 56·8 to 190 Kyr. The problem of chronology of Palaeolithic artifacts is interlinked with the miliolite and other coastal formations. The present investigations permit the development of a chronological framework for the Palaeolithic cultures in the Hiran Valley in particular, and generally in Saurashtra Peninsula. On the basis of radiometric dates and relative chronology, the Lower Palaeolithic cultures fall in a time-bracket of 190-69 Kyr bp. The Middle Palaeolithic industry is much older than 56·8 Kyr bp. The dates obtained for the Lower Palaeolithic cultures are perhaps the oldest reported to date.     

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.     

A SIMPLE FIELD KIT FOR IDENTIFYING C4 PLANTS*

We have developed a simple field kit for identifying C₄ plants, the use of which requires little technical training. The system has proven very useful for surveying plants in areas for which carbon isotopic dating and dietary studies are to be undertaken.     

ATTENUATION RELATIONSHIP FOR LOW MAGNITUDE EARTHQUAKES USING STANDARD SEISMOMETRIC RECORDS

Northwestern Italian weak-motion data were used to study attenuation characteristics of horizontal peak ground acceleration (PGA) and horizontal peak ground velocity (PGV) from earthquakes of local magnitudes (M _l ) up to 5.1. Data have been provided by the RSNI (Regional seismic network of Northwestern Italy) and RSLG (Regional seismic network of Lunigiana-Garfagnana) waveform database. The database consists of more than 14000 horizontal components recorded in the period 1999-2002 by both broadband and enlarged band seismometers. The accuracy of the procedure used to extract PGA values from the velocity recordings was verified comparing observed and derived PGA values at station STV2, which was equipped with both a temporary K2 Kinemctrtcs accelerometer and Guralp CMG40 broadband sensor. The attenuation of both peak ground acceleration and peak ground velocity was found to be logarithmically distributed with a strong attenuation for low distances (less than 50 km) and low M _l values (<3.0). The resulting equations are:

Log(PGA)=?3.19+0.87M?0.042M ²?1.92 Log(R)+0.249S,

Log(PGA)=?4.23+0.76M?0.018M²?1.56 Log(R)+0.230S,

where PGA is expressed in g, PGV is expressed in m/s, M is local magnitude, R is the hypocentral distance in kilometers and S is a dummy variable assuming values of 0 and 1 for rock and soil respectively. For increasing distance and magnitude, both PGA and PGV values show a linear distribution. The validity range of the obtained attenuation relationships is 0–200 km for distances and M _l up to 4.5. Sensitivity studies performed by analysis of residuals, showed that predicted PGA and PGV values are stable with respect to reasonable variations of the model and distances providing the data. Comparisons with attenuation relationships proposed for Italian region, derived from strong motion records, are also presented.     

ISSUES RELATED TO DETERMINING BURIAL CHRONOLOGY BY FLUORIDE ANALYSIS OF BONE FROM THE MAYA ARCHAEOLOGICAL SITE OF CHAU HIIX,BELIZE*

Fluoride percentage of bone is often used to determine relative dates of burials in archaeological contexts. An analysis of prehistoric Maya burials at Chau Hiix, Belize, identifies taphonomic factors, including soil composition, grave depth, soil disturbance, age at death and cortical bone thickness, that cause variations in the rate of fluoride absorption by altering the access of water to bone. This example demonstrates that fluoride dating is unlikely to be useful at most prehistoric Maya sites because of the inconsistent taphonomy due to typically diverse mortuary practices, and it also serves as a cautionary tale for applications of this methodology in other contexts.     

A NEW DIRECT RADIOCARBON AMS DATE FOR AN UPPER PALAEOLITHIC HUMAN BONE FROM SIBERIA

A new AMS radiocarbon date has been obtained from a Siberian human bone sample taken directly from a cranial fragment. The specimen comes from the north‐east Siberian site of Pokrovka 2 (55⁰19′46.30″N, 92⁰26′48.80″E). The remains consist of the anterior portion of the cranium or the superior part of the face; that is, the forehead and the roof of the eye sockets. Sadly, indifferent features of the frontal bone do not allow a confident diagnosis of the sex of the individual. The evidence suggests, however, that the remains are probably those of a young adult (teenager) and an anatomically modern human, rather than a Neanderthal. Radiocarbon dating was undertaken at the Oxford Radiocarbon Accelerator Unit (ORAU). The radiocarbon age determination of the bone fragment, 27 740 ± 150 bp (OxA‐19850), is one of the earliest direct dates for a modern human from Siberia. The Pokrovka cranial fragment dates to the middle Upper Palaeolithic of Eurasia and is broadly contemporary with the human remains from the famous eastern European site of Sunghir. When the radiocarbon age is compared with the Cariaco Basin ¹⁴C data set and the Greenland oxygen isotope record of NGRIP, it corresponds with Greenland Interstadial 5, a warmer phase of the Last Glacial period, although this is a preliminary conclusion, and is based on climate records that may or may not be wholly synchronous between the two locations.     

METHODOLOGICAL DEVELOPMENTS IN THE LUMINESCENCE DATING OF BRICK FROM ENGLISH LATE‐MEDIEVAL AND POST‐MEDIEVAL BUILDINGS*

Fired clay brick samples, obtained from a group of seven high‐status late‐medieval and post‐medieval buildings in England ranging in age from c. ad 1390 to 1740, were dated by the luminescence method using an optically stimulated luminescence (OSL) technique. The results obtained indicate that, when applied to quartz extracted from brick, the technique is capable of producing dates that are in consistently good agreement with independent dating evidence for the buildings. For six samples taken from a group of four dating ‘control’ buildings the mean difference between the central values of luminescence and assigned ages was 5 ± 10 years (SD, n = 6). The methodology used is appropriate for application to other standing buildings in other temporal and geographic regions, and may be used with confidence where conventional dating methods are less certain. The study also examines the luminescence characteristics of quartz and the characteristics of the lithogenic radionuclides in brick samples and identifies various aspects related to the assessment of experimental uncertainty in testing the reliability of the method.