Rehydroxylation of Fired‐Clay Ceramics: Factors Affecting Early‐Stage Mass Gain in Dating Experiments

To obtain accurate results in the RHX dating of ceramics, it is essential that the RHX measurements are continued until the rate of mass gain is constant with (time)^1/4. In this paper, we discuss how the initial stages of mass gain are affected by the specific surface area (SSA) of the ceramic material. The paper provides guidance on experimental protocols to avoid dating results being distorted by relatively early‐time mass gain data.     

The influence of temperature on rehydroxylation [RHX] kinetics in archaeological pottery

Almost all archaeological ceramics undergo slow, progressive rehydroxylation by chemical combination with environmental water. The reaction is accompanied by an expansion, and also by the small but measurable mass gain that provides the basis of the RHX dating method. The rate of the RHX reaction increases with increasing temperature. Here we describe comprehensively the effects of temperature on the RHX process in relation to the dating methodology. We deal in turn with the kinetic model of the RHX reaction, the temperature dependence of the RHX rate, and the influence of varying environmental temperature on the RHX mass gain. We define an effective lifetime temperature and show how this is calculated from an estimated lifetime temperature history. Historical meteorological temperature data are used to estimate the lifetime temperature history, and this can be adjusted for long-term climate variation. We show also how to allow for the effects of burial in archaeological sites on the temperature history. Finally we describe how the uncertainties in estimates of RHX age depend on the estimates of temperature history and effective lifetime temperature.     

Pottery firing temperatures: a new method for determining the firing temperature of ceramics and burnt clay

A new method for determining the maximum firing temperature of ceramics and burnt clay is presented. The technique relies on measuring the magnetic susceptibility on a step-wise re-fired sample. The validity of the method has been tested by determining firing temperatures of two sets of clay samples fired at temperatures ranging from 400 to 1000 °C. Aliquots of the same samples have been studied petrographically by optical microscopy on thin sections and analyzed by powder X-ray diffraction in order to monitor structural and mineralogical changes as a function of temperature. The method is demonstrated on samples from four geographically widely different sites and it is applied to a larger set of ceramics of Late (ca. AD 900–AD 1450) and Inca (ca. AD 1480–AD 1532) periods from the Northwestern Argentine region, dating to a limited period of time prior to the fall of the Inca Empire. The method is shown to be a powerful tool in revealing archaeological information about the change in firing technologies in the pre-Hispanic societies in the Andean area through time.     

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.     

The archaeology of radiocarbon accelerator dating

Accelerator mass spectrometry (AMS) allows radiocarbon dating to be carried out by direct counting of¹⁴C atoms, rather than the conventional counting of radioactive disintegrations. The result is that samples up to 1000 times smaller can be handled. The approach was tested in principle by 1977 and for archaeological operation by 1983. More than 2000 samples per year are now being dated worldwide. The machines can now operate to about ± 80 years or better. Dates older than 40,000 years have not yet been achieved, but the ability to use small samples has already had considerable impact on dating the period 10,000–30,000 years ago. Bone is an ideal material for the new technique, since amino acids can normally be isolated and purified from gram-size samples. Studies of the origins of domestication are aided by the dating of individual grains and seeds. Because small samples can be mobile in the soil, careful sample selection strategies and procedures are required. The full impact of the technique can be assessed only through the rapid and comprehensive publication of archaeological results.     

Radiocarbon dating and the “old shell” problem: direct dating of artifacts and cultural chronologies in coastal and other aquatic regions

Archaeologists have long recognized the problem of the “old wood” effect in radiocarbon dating charcoal and wood samples, the age of which may be hundreds of years older than their use by humans. Such problems have resulted in significant changes in how most researchers select wood and charcoal samples for ¹⁴C dating, with many now using relatively short-lived carbonized materials for dating. Despite the significant strides made in our understanding of the potential biases of the “old wood” effect, little emphasis has been placed on the possible impacts of dating “old shell” in archaeological deposits. The use of marine shell for ¹⁴C dating is widespread in coastal areas around the world, including a growing emphasis on the dating of individual shell artifacts via Accelerator Mass Spectrometry (AMS). In dating shell artifacts, we have obtained several dates older than associated ¹⁴C dates for short-lived subsistence remains from the same deposits, including great disparities (>10,000 years) and more subtle differences (≥100 years). These discrepancies appear to be due to the use of old shells by humans to make beads and other artifacts, including shells collected from fossil deposits, older archaeological sites, and beaches. The problems caused by the use of old shells to make beads and other artifacts are surmountable through careful sample selection, analysis of multiple ¹⁴C dates on a variety of materials, and proper calibration procedures.     

First dendroarchaeological dates of prehistoric contexts in South America: chullpas in the Central Andes

Despite the existence of long-lived tree species with excellent tree-ring characteristics, the use of dendrochronological techniques for dating archaeological contexts has been very limited in South America. Recent research in the Bolivian Altiplano of the Central Andes has yielded a network of Polylepis tarapacana chronologies that goes back to the 13th century. This species was regularly used by local populations since pre-Columbian times as raw material for beams, lintels, hooks and other architectural features in houses, storage chambers, and sepulchers. The aim of this study is to argue in favor of the potential of P. tarapacana for providing high resolution dates of significant archaeological events during the pre-Columbian era. The chronology of chullpas (burial towers and storage chambers) in the southern Andean Altiplano is used as a case study. Growth rings from P. tarapacana have provided several centennial-length dendrochronological records including a reference regional chronology covering the last 786 years in the Central Andean highlands. Based on this long reference chronology calendar years were assigned to woody pieces from pre-Hispanic chullpas. Dendroarchaeological results are consistent with contextual evidence and most radiocarbon dates from woody samples and related archaeological items. Our results indicate that P. tarapacana has a high potential for providing annually-resolved tree-ring dates for archaeological contexts in the Altiplano since the early 13th century.     

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.     

THE USE OF TRACE ELEMENT ANALYSIS OF ENTRAPPED SLAG INCLUSIONS TO ESTABLISH ORE – BAR IRON LINKS: EXAMPLES FROM TWO GALLO‐ROMAN IRON‐MAKING SITES IN FRANCE (LES MARTYS,MONTAGNE NOIRE,AND LES FERRYS,LOIRET)*

Knowledge of the iron trade in ancient times rests on determining the source of the objects recovered during archaeological excavations. Unfortunately, attributing the origin is not always possible using archaeological tools alone. Trace element data of the ore and the archaeological material (reduction and reheating slags, entrapped slag inclusions from the bloom, bar iron and iron blades) from two Gallo‐Roman iron‐making centres, Les Martys (Montagne Noire) and Les Ferrys (Loiret), were determined using ICP–AES/MS and LA–ICP–MS. The results highlight a continuity of composition that makes it possible to establish a link between the initial ore and the semi‐finished iron products.     

Dating problems in Icelandic archaeology

For many decades tephrochronology has been used as a scientific method for dating archaeological as well as geological remains in Iceland. Recently, parts of the tephrochronology for the eruptions of the famous volcano Hekla have been questioned by the author. This is due to obvious differences in dating results of archaeological artefacts from the valley of Thjórsárdalur in southern Iceland and the current tephrochronological dating of its devastation. While the devastation of the valley has been dated to AD 1104 and is thought to have been caused by a huge eruption of mount Hekla in that year, the artefacts from excavations and stray finds, as well as new ¹⁴C results, show somewhat later 12th‐13th century dates. The paper deals with this obvious discrepancy, which has hitherto been ignored, together with the results of archaeological excavations in 1983–86 at Stóng in Thjórsárdalur; it also gives a critical analysis of the historical methodology of the tephrochronologists.     

Implications of a freshwater radiocarbon reservoir correction for the timing of late Holocene settlement of the Elk Hills,Kern County,California

Uncertainties regarding the magnitude of freshwater radiocarbon reservoir effects can introduce random errors into dates on archaeological freshwater carbonates. As a result, many archaeologists avoid dating freshwater shells unless no other datable materials are available. The chronology of prehistoric occupation of the former Naval Petroleum Reserve No. 1 (NPR-1) at Elk Hills, Kern County, has been established with 50 radiocarbon dates on freshwater mussels (Gonidea and Anodonta sp.). Characterization of any freshwater radiocarbon reservoir effect is crucial for the accurate interpretation of inferred settlement and subsistence changes on the Elk Hills. Paired charcoal and freshwater mussels sampled from closely associated contexts were dated to identify a freshwater reservoir effect. Paired Anodonta and Gonidea sp. shells were dated to investigate interspecific differences in fractionation. Results indicate that a 340 ± 20 ¹⁴C yr correction should be applied to conventional ¹⁴C dates on freshwater carbonates in the Buena Vista Basin before calendar calibration. Evidence of interspecific differences is inconclusive. Dates recalibrated with the reservoir correction indicate that widespread occupation of the Elk Hills is correlated with increasing precipitation towards the end of the Medieval Climatic Anomaly and during the Little Ice Age, suggesting that slough resource exploitation may have been driven by regional population pressure rather than drought-related declines in aquatic productivity.     

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.     

Microchemical and crystallographic analysis of human bones from Nasca,Peru. A possible method of direct dating of archaeological skeletal material

This paper provides two archaeometric equations obtained by crystal–chemical parameters for dating human bone samples from the archaeological site of Nasca, Peru. Based on radiocarbon dating, the burials span from 500 BC to AD 1000. Crystal–chemical modifications in bone hydroxylapatite over time were compared with a twentieth century skeleton from Italy. Chemical analysis was carried out by means of electron microprobe along a profile from the periosteal to the endosteal border of the midshaft of four human femurs. The results indicate that the Ca/P ratio is linearly correlated with time according to the equation t=7880.68Ca/P−12805.90 (r=0.97; r²=0.95). Bone apatite X-ray powder diffraction analysis showed a systematic increase in the (002) reflection intensity with time, according to the equation t=250.49h/a−1961.86 (r=0.98; r²=0.97). The two independent archaeometric equations permit good accuracy in dating osteoarchaeological remains from the south coast area of Peru. © 1998 John Wiley & Sons, Ltd.     

Dietary change in Fijian prehistory: isotopic analyses of human and animal skeletal material

We examine evidence for prehistoric diet in the Fiji Islands through the analysis of stable isotope ratios (δ¹³C and δ¹⁵N) for 26 samples of human and animal bones from various archaeological sites, time periods, and local environments. The oldest individuals in this study, dating to about 2700 BP and living on the small island of Waya, consumed a predominantly marine-based diet. Subsequent populations on this island showed reduced consumption of marine resources, with greater reliance on terrestrial ones, throughout the cultural sequence. In contrast, populations of humans and pigs living inland on Viti Levu, the largest island, relied on terrestrial resources since at least 1500 BP. Thus, our results suggest that human and pig diets throughout Fijian prehistory relied variably on marine or terrestrial resources, and this distinction is largely a product of geography. This finding and our analyses provide a model for understanding ancient diets in Remote Oceania.     

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.     

An archaeologically validated protocol for computing obsidian hydration rates from laboratory data

This paper reports the computation of hydration rate for Topaz Mountain obsidian from laboratory data, and a comparison with archaeological data from a well-dated site, Camels Back Cave, in western Utah. Topaz Mountain obsidian is found to be slow-hydrating, with a rate of 0.071 ± 0.021 μ/yr^½ at an effective hydration temperature of 16.01 °C. This rate agrees with a rate developed from archaeological data from Camels Back Cave within ∼6%. Activation energy of Topaz Mountain obsidian is 10370 ± 544 K, and its diffusion constant is (1.87 ± 9.13) × 10¹³ μ²/yr, both of which are independent of temperature. Its intra-source variability in hydration rate is very low (CV < 0.01), implying a low variability in intrinsic water. We present a model of chemical erosion which shows why earlier laboratory-determined rates were incorrect, and discuss the implications of our findings on the determination of experimentally derived rates in obsidian hydration dating.     

The Baelo Claudia Paradigm: The Exploitation of Marine Resources in Roman Cetariae

The Roman city of Baelo Claudia (Baetica, Hispania) is one of the best known halieutic sites of the Mare Nostrum, dating from between the 2nd century BC and the 5th century AD. Recent archaeological investigations have included the discovery, excavation and interdisciplinary study of two new fish-salting factories (so-called “Conjuntos Industriales” XI and XII), providing valuable new information on the exploitation of marine resources. This paper provides the first synthesis of all of the available archaeological evidence for the first three phases of the fishing-product cycle (marine resources/fishing equipment/processing facilities and food products) at this unique site on the Strait of Gibraltar.     

Calcium oxalate AMS C dating and chronology of post-Palaeolithic rock paintings in the Iberian Peninsula. Two dates from Abrigo de los Oculados (Henarejos,Cuenca, Spain)

Since 2005 we have been utilizing accelerator mass spectrometry (AMS) ¹⁴C dating in research on calcium oxalate crusts associated with open air rock art of the Iberian Peninsula. In this paper we present two dates linked with three eye-idol pictographs at Abrigo de los Oculados (Henarejos, Cuenca, Spain). Radiocarbon ages for these motifs agree with the expected iconography-based archaeological chronology. Such oxalate dates could provide an independent basis for evaluating chronological theories for post-Palaeolithic sites, designated in the UNESCO World Heritage List as Rock Art of the Mediterranean Basin on the Iberian Peninsula.     

Palaeoenvironmental significance of grain-size distribution of river flood deposits: a study of the archaeological sites of the Apengjiang River Drainage,upper Yangtze region,Chongqing, China

The grain-size distribution (based on cumulative probability curves) in the sediments produced by potential palaeofloods at the Shiniusi archaeological site is similar to that of modern flood sediments from the Wujiang River Drainage in the upper Yangtze River. There is an obvious pattern in the curves, with two segments, and the mean grain size (Mz), standard deviations (σ1), skewness, and kurtosis are all similar. Combined with the AMS¹⁴C dating data and the ages judged based on the presence of cultural remains, our data suggests frequent palaeoflood events within the Wujiang River Drainage. We hypothesize the existence of seven high flood possibility layers in the QST4 unit from Shiniusi archaeological site: during the periods of the Ming Dynasty (1368–1644 AD) to the Qing Dynasty (1616–1911 AD), and the end of the Eastern Zhou Dynasty (770 BC–256 BC) to the Shang Dynasty (1600–1100 BC). We also hypothesize ten high flood probability layers in the QST2 unit from Shiniusi archaeological site: during the periods of the Ming Dynasty to the Qing Dynasty, the periods of Song Dynasty (960–1279 AD) to the Yuan Dynasty (1206–1368 AD), as well as during the Han Dynasty (207 BC–220 AD) to the Eastern Zhou Dynasty (770 BC–256 BC). These results are consistent with palaeoflood events inferred from pollen and spore analysis and from historical records in other rivers.     

Red abalone collecting and marine water temperature during the Middle Holocene occupation of Santa Cruz Island,California

Oxygen isotope values derived from prehistoric mussel (Mytilus californianus) shell calcite are used to determine whether sea-surface temperatures in the vicinity of the Punta Arena site (CA-SCRI-109) on Santa Cruz Island, California, were cooler than present between 6300 and 5300 cal BP. This site and others in the western sector of the island dating to this period are distinctive because of the presence of large red abalone (Haliotis rufescens) shells, a species that historically has been subtidal around Santa Cruz and the other northern Channel Islands. Comparison of temperature values derived from archaeological shells with those from modern mussel shells, along with water temperatures derived from satellites, indicates that waters were cooler during the 6300 to 5300 cal BP period. These results are consistent with a previous study and support the interpretation that collection of red abalone during the 6300–5300 cal BP period was partly the result of cooler water temperatures that made this large mollusk more available to foragers in the intertidal or shallow subtidal zone.