Accurate compound-specific 14C dating of archaeological pottery vessels.

Pottery is one of the most commonly recovered artefacts from archaeological sites. Despite more than a century of relative dating based on typology and seriation1, accurate dating of pottery using the radiocarbon dating method has proven extremely challenging owing to the limited survival of organic temper and unreliability of visible residues2-4. Here we report a method to directly date archaeological pottery based on accelerator mass spectrometry analysis of 14C in absorbed food residues using palmitic (C16:0) and stearic (C18:0) fatty acids purified by preparative gas chromatography5-8. We present accurate compound-specific radiocarbon determinations of lipids extracted from pottery vessels, which were rigorously evaluated by comparison with dendrochronological dates9,10 and inclusion in site and regional chronologies that contained previously determined radiocarbon dates on other materials11-15. Notably, the compound-specific dates from each of the C16:0 and C18:0 fatty acids in pottery vessels provide an internal quality control of the results6 and are entirely compatible with dates for other commonly dated materials. Accurate radiocarbon dating of pottery vessels can reveal: (1) the period of use of pottery; (2) the antiquity of organic residues, including when specific foodstuffs were exploited; (3) the chronology of sites in the absence of traditionally datable materials; and (4) direct verification of pottery typochronologies. Here we used the method to date the exploitation of dairy and carcass products in Neolithic vessels from Britain, Anatolia, central and western Europe, and Saharan Africa.

The importance of shell: Redating of the To'aga site (Ofu Island, Manu'a) and a revised chronology for the Lapita to Polynesian Plainware transition in Tonga and Samoa.

Radiocarbon dating Pacific archaeological sites is fraught with difficulties. Often situated in coastal beach ridges or sand dunes, these sites exhibit horizontal and vertical disturbances, datable materials such as wood charcoal are typically highly degraded, may be derived from old trees or driftwood unless specifically identified to short-lived material, while bone collagen rarely survives in tropical conditions. Shell, therefore, is the most logical material for dating Pacific sites since it is resistant to alteration, can be sampled to ensure only the last few seasons of growth are represented and is often closely tied to human economic activities. However, shell radiocarbon (14C) dating has been plagued by interpretive problems largely due to our limited knowledge of the 14C cycle in nearshore marine and estuarine environments. Consequently, shell dates are typically ignored in regional chronometric evaluations and in recent years shell is often avoided for dating altogether. Recent advances in our understanding of the source of shell 14C as well as the development of the first South Pacific Gyre model of changing marine 14C over time, combined with Bayesian statistical modelling, now provide us with insight into the value of these shell radiocarbon dates. Here we present a revision of the age of the To'aga site on Ofu Island-an early occupation site associated with the initial Polynesian Plainware period in Samoa, the earliest use of which we date to between 2785 and 2607 cal BP (68% probability).

Empirical calibrated radiocarbon sampler: a tool for incorporating radiocarbon-date and calibration error into Bayesian phylogenetic analyses of ancient DNA.

Studies of DNA from ancient samples provide a valuable opportunity to gain insight into past evolutionary and demographic processes. Bayesian phylogenetic methods can estimate evolutionary rates and timescales from ancient DNA sequences, with the ages of the samples acting as calibrations for the molecular clock. Sample ages are often estimated using radiocarbon dating, but the associated measurement error is rarely taken into account. In addition, the total uncertainty quantified by converting radiocarbon dates to calendar dates is typically ignored. Here, we present a tool for incorporating both of these sources of uncertainty into Bayesian phylogenetic analyses of ancient DNA. This empirical calibrated radiocarbon sampler (ECRS) integrates the age uncertainty for each ancient sequence over the calibrated probability density function estimated for its radiocarbon date and associated error. We use the ECRS to analyse three ancient DNA data sets. Accounting for radiocarbon-dating and calibration error appeared to have little impact on estimates of evolutionary rates and related parameters for these data sets. However, analyses of other data sets, particularly those with few or only very old radiocarbon dates, might be more sensitive to using artificially precise sample ages and should benefit from use of the ECRS.

Radiometric 81Kr dating identifies 120,000-year-old ice at Taylor Glacier, Antarctica.

We present successful (81)Kr-Kr radiometric dating of ancient polar ice. Krypton was extracted from the air bubbles in four ∼350-kg polar ice samples from Taylor Glacier in the McMurdo Dry Valleys, Antarctica, and dated using Atom Trap Trace Analysis (ATTA). The (81)Kr radiometric ages agree with independent age estimates obtained from stratigraphic dating techniques with a mean absolute age offset of 6 ± 2.5 ka. Our experimental methods and sampling strategy are validated by (i) (85)Kr and (39)Ar analyses that show the samples to be free of modern air contamination and (ii) air content measurements that show the ice did not experience gas loss. We estimate the error in the (81)Kr ages due to past geomagnetic variability to be below 3 ka. We show that ice from the previous interglacial period (Marine Isotope Stage 5e, 130-115 ka before present) can be found in abundance near the surface of Taylor Glacier. Our study paves the way for reliable radiometric dating of ancient ice in blue ice areas and margin sites where large samples are available, greatly enhancing their scientific value as archives of old ice and meteorites. At present, ATTA (81)Kr analysis requires a 40-80-kg ice sample; as sample requirements continue to decrease, (81)Kr dating of ice cores is a future possibility.

Dating human bone: is racemization dating species-specific?

Our recently developed dating technique based on the racemization rate of aspartic acid was applied to dating human bone, as well as that of other mammals, utilizing capillary electrophoresis mass spectrometry. First, several well-dated (mostly (14)C-dated and with strong archeological evidence) human bones ranging in age from 150 to ~10,000 years were used to develop a calibration curve for human bone. The D/L ratio of aspartic acid for these specimens ranged from 2.4% to ~10%, with a correlation coefficient of better than 0.99, indicating a strong linear relationship between the d/l ratio of aspartic acid and the age of the specimens. This calibration curve can now be used to date human archeological specimens of unknown age, up to ~10,000 years. However, when the technique was applied to well-dated mixed species of larger mammal bones such as bison, whale, llama, etc., the calibration curve showed a slower rate of racemization with a lower correlation (0.88). As additional large mammal bones with less certain age (i.e., using archeological evidence alone with no (14)C-dating) were dated the correlation coefficient decreased to 0.70. The correlation coefficient decreased further to 0.58 when the racemization data from all mammals (including human) were added to the calibration curve, indicating the importance of using well-dated, species-specific specimens for forming a calibration curve. This conclusion is consistent with our previously published calibration curve for a single species of silk (Bombyx mori), which followed the expected reversible first-order kinetics. These results support species specificity of amino acid racemization dating.

A complete terrestrial radiocarbon record for 11.2 to 52.8 kyr B.P.

Radiocarbon ((14)C) provides a way to date material that contains carbon with an age up to ~50,000 years and is also an important tracer of the global carbon cycle. However, the lack of a comprehensive record reflecting atmospheric (14)C prior to 12.5 thousand years before the present (kyr B.P.) has limited the application of radiocarbon dating of samples from the Last Glacial period. Here, we report (14)C results from Lake Suigetsu, Japan (35°35'N, 135°53'E), which provide a comprehensive record of terrestrial radiocarbon to the present limit of the (14)C method. The time scale we present in this work allows direct comparison of Lake Suigetsu paleoclimatic data with other terrestrial climatic records and gives information on the connection between global atmospheric and regional marine radiocarbon levels.

At the end of the 14C time scale--the Middle to Upper Paleolithic record of western Eurasia.

The dynamics of change underlying the demographic processes that led to the replacement of Neandertals by Anatomically Modern Humans (AMH) and the emergence of what are recognized as Upper Paleolithic technologies and behavior can only be understood with reference to the underlying chronological framework. This paper examines the European chronometric (mainly radiocarbon-based) record for the period between ca. 40 and 30 ka 14C BP and proposes a relatively rapid transition within some 2,500 years. This can be summarized in the following falsifiable hypotheses: (1) final Middle Paleolithic (FMP) "transitional" industries (Uluzzian, Chatelperronian, leaf-point industries) were made by Neandertals and date predominantly to between ca. 41 and 38 ka 14C BP, but not younger than 35/34 ka 14C BP; (2) initial (IUP) and early (EUP) Upper Paleolithic "transitional" industries (Bachokirian, Bohunician, Protoaurignacian, Kostenki 14) will date to between ca. 39/38 and 35 ka 14C BP and document the appearance of AMH in Europe; (3) the earliest Aurignacian (I) appears throughout Europe quasi simultaneously at ca. 35 ka 14C BP. The earliest appearance of figurative art is documented only for a later phase ca. 33.0/32.5-29.2 ka 14C BP. Taken together, the Middle to Upper Paleolithic transition appears to be a cumulative process involving the acquisition of different elements of "behavioral modernity" through several "stages of innovation."

The Middle to Upper Paleolithic transition: dating, stratigraphy, and isochronous markers.

Accurate and precise dating is vital to our understanding of the Middle to Upper Paleolithic transition. There are, however, a number of uncertainties in the chronologies currently available for this period. We attempt to examine these uncertainties by utilizing a number of recent developments in the field. These include: the precise dating of the Campanian Ignimbrite (CI) tephra by 40Ar/39Ar; the tracing of this tephra to a number of deposits that are radiocarbon dated; the publication of revised radiocarbon calibration data for the period, showing a much better convergence with other available data than during the recent IntCal comparison; and a layer-counted ice-core chronology extending beyond 40,000cal BP. Our data comparisons suggest that a reasonable overall convergence between calibrated radiocarbon ages and calendar dates is possible using the new curves. Additionally, we suggest that charcoal-based radiocarbon ages, as well as bone-based radiocarbon determinations, require cautious interpretation in this period. Potentially, these issues extend far beyond the sites in this study and should be of serious concern to archaeologists studying the Middle to Upper Paleolithic. We conclude by outlining a strategy for moving the science forward by a closer integration of archaeology, chronology, and stratigraphy.

Radiocarbon dating the late Middle Paleolithic and the Aurignacian of the Swabian Jura.

Many lines of evidence point to the period between roughly 40 and 30 ka BP as the period in which modern humans arrived in Europe and displaced the indigenous Neandertal populations. At the same time, many innovations associated with the Upper Paleolithic--including new stone and organic technologies, use of personal ornaments, figurative art, and musical instruments--are first documented in the European archaeological record. Dating the events of this period is challenging for several reasons. In the period about six to seven radiocarbon half-lives ago, variable preservation, pre-treatment, and sample preparation can easily lead to a lack of reproducibility between samples and laboratories. A range of biological, cultural, and geological processes can lead to mixing of archaeological strata and their contents. Additionally, some data sets point to this period as a time of significant spikes in levels of atmospheric radiocarbon. This paper assesses these questions in the context of the well-excavated and intensively studied caves of Geissenklösterle and Hohle Fels in the Swabian Jura of southwestern Germany. We conclude that variable atmospheric radiocarbon production contributes to the problems of dating the late Middle Paleolithic and the early Upper Paleolithic. To help establish a reliable chronology for the Swabian Aurignacian, we are beginning to focus our dating program on short-lived, stratigraphically secure features to see if they yield reproducible results. This approach may help to test competing explanations for the noisy and often non-reproducible results that arise when trying to date the transition from the Middle to the Upper Paleolithic.

Art and the Middle-to-Upper Paleolithic transition in Europe: comments on the archaeological arguments for an early Upper Paleolithic antiquity of the Grotte Chauvet art.

The spectacular art of the Grotte Chauvet stands out among all other examples of Aurignacian art, which are restricted to a handful of sites in other regions of western and Central Europe, which take the form of sophisticated carvings on organic materials and of simple engravings on rockshelter walls. Given its sophistication, Chauvet has understandably come to feature prominently in debates as to the nature of human symbolic origins, the behavioral capacities of Homo sapiens, the nature of the dispersal of modern humans across Europe, and the possibly contemporary extinction of Homo neanderthalensis. Significant objections to such an antiquity have, however, been made in recent years on the grounds of the style, themes, and technical practice of the art itself, and on the grounds of the AMS radiocarbon dating program that was first seen to suggest an early Upper Paleolithic age. To date, no attention has been paid to claims for an Aurignacian age on specifically archaeological grounds. Here, I undertake a critical examination of the archaeology of the cave and its wider region, as well as attempts to verify the antiquity of the art on the basis of comparison with well-dated Aurignacian art elsewhere. I conclude that none of the archaeological arguments withstand scrutiny and that many can be rejected as they are either incorrect or tautologous. By contrast, hypotheses that the art is of Gravettian-Magdalenian age have not been successfully eliminated. The age of the art of the Grotte Chauvet should be seen as a scientific problem, not an established fact. While it may prove impossible to prove an Aurignacian age for some of the Chauvet art I suggest a set of expectations that would, in combination, strengthen the robusticity of the 'long chronology' argument. The onus is upon Chauvet long chronologists to do this, and until they do, we must conclude that the art of the Grotte Chauvet is not dated, and very possibly much younger than claimed.