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Radiocarbon (14C) ages cannot provide absolutely dated chronologies for archaeological or paleoenvironmental studies directly but must be converted to calendar age equivalents using a calibration curve compensating for fluctuations in atmospheric 14C concentration. Although calibration curves are constructed from independently dated archives, they invariably require revision as new data become available and our understanding of the Earth system improves. In this volume the international 14C calibration curves for both the Northern and Southern Hemispheres, as well as for the ocean surface layer, have been updated to include a wealth of new data and extended to 55,000 cal BP. Based on tree rings, IntCal20 now extends as a fully atmospheric record to ca. 13,900 cal BP. For the older part of the timescale, IntCal20 comprises statistically integrated evidence from floating tree-ring chronologies, lacustrine and marine sediments, speleothems, and corals. We utilized improved evaluation of the timescales and location variable 14C offsets from the atmosphere (reservoir age, dead carbon fraction) for each dataset. New statistical methods have refined the structure of the calibration curves while maintaining a robust treatment of uncertainties in the 14C ages, the calendar ages and other corrections. The inclusion of modeled marine reservoir ages derived from a three-dimensional ocean circulation model has allowed us to apply more appropriate reservoir corrections to the marine 14C data rather than the previous use of constant regional offsets from the atmosphere. Here we provide an overview of the new and revised datasets and the associated methods used for the construction of the IntCal20 curve and explore potential regional offsets for tree-ring data. We discuss the main differences with respect to the previous calibration curve, IntCal13, and some of the implications for archaeology and geosciences ranging from the recent past to the time of the extinction of the Neanderthals.
Subfossil trees with their annual rings constitute the most accurate and precise archive to calibrate the radiocarbon (14C) method. The Holocene part of the IntCal curve is based on tree-ring chronologies, absolutely dated by dendrochronological matching. For the Northern Hemisphere, the absolute curve starts at 12,325 cal BP. For the early part of the Younger Dryas (YD) climatic event (≈ 12,850–11,650 cal BP), there are only a few floating dendrochronological sequences, mainly from Switzerland and France. We present new 14C results from subfossil trees (Pinus sylvestris L.) collected from the Barbiers site (southeast French Alps). The dendrochronological series covers 416 years, corresponding to the onset of the YD period. In order to date our sequence, we matched it with the 14C record based on kauri trees from New Zealand. The Barbiers data were first averaged at the same decadal resolution as the kauri record. Statistical comparison of the different averaging options and matching techniques enables dating the Barbiers sequence to 13,008–12,594 ±10 cal BP, which thus includes the boundary between the Allerød and YD events. The new Barbiers record allows to calculate the 14C inter-hemispheric gradient (14C-IHG) during the period overlapping the kauri sequence. For the optimal dating option, the mean 14C-IHG is 37 yr with a standard deviation (SD) of 21 yr based on 43 decadal estimations (−6‰ with SD of 2‰). The 14C-IHG record exhibits minimal values, down to zero, between 12,960–12,840 cal BP. Excluding these minima leads to an average 14C-IHG of 45 yr with a SD of 14 yr based on 33 decadal values, in agreement with observations for the last two millennia. The Barbiers record suggests a 14C-IHG increase between the end of the Allerød period (IHG of 37 yr with SD of 14 yr) and the early part of the YD (IHG of 48 yr with SD of 14 yr), which is compatible with previously reported drop of deep-water convection in the North-Atlantic and the associated increase in wind-driven upwelling in the Southern Ocean.
To date, finding a technique able to effectively isolate the carbon signal from the binder of a mortar is still an open challenge. In this paper, the radiocarbon (14C) dating of one of the most challenging and diffuse types of mortar, the one with pozzolana aggregate, is investigated. Eight mortar samples from three archaeological sites near Rome (Italy) underwent a selection process called Cryo2SoniC. The selected fractions were analyzed by the accelerator mass spectrometry (AMS) 14C technique and compared to known historical references. Additional scanning electron microscopy analysis and petrographic investigations were done, respectively, to check the grain size of the fractions selected by Cryo2SoniC, and further, to characterize the original mortar samples. The masses of carbon yielded from the dated fractions were almost half of those released from some aerial mortars. The 14C dating results were accurate for pozzolana mortars, from buried and unburied structures, with calcination relics and small contamination of secondary calcite. A limitation in the purification protocol was observed on samples with a massive contamination of secondary calcite deposition of ground water origin, occluding porosity and substituting up to the 80% of the original binder matrix.
Absolute dating of mortars is crucial when trying to pin down construction phases of archaeological sites and historic stone buildings to a certain point in time or to confirm, but possibly also challenge, existing chronologies. To evaluate various sample preparation methods for radiocarbon (14C) dating of mortars as well as to compare different dating methods, i.e. 14C and optically stimulated luminescence (OSL), a mortar dating intercomparison study (MODIS) was set up, exploring existing limits and needs for further research. Four mortar samples were selected and distributed among the participating laboratories: one of which was expected not to present any problem related to the sample preparation methodologies for anthropogenic lime extraction, whereas all others addressed specific known sample preparation issues. Data obtained from the various mortar dating approaches are evaluated relative to the historical framework of the mortar samples and any deviation observed is contextualized to the composition and specific mineralogy of the sampled material.
Seven radiocarbon laboratories: Åbo/Aarhus, CIRCE, CIRCe, ETHZ, Poznań, RICH, and Milano-Bicocca performed separation of carbonaceous fractions suitable for 14C dating of four mortar samples selected for the MOrtar Dating Inter-comparison Study (MODIS). In addition, optically stimulated luminescence (OSL) analyses were completed by Milano-Bicocca and IRAMAT-CRP2A Bordeaux. Each laboratory performed separation according to laboratory protocol. Results of this first intercomparison show that even though consistent 14C ages were obtained by different laboratories, two mortars yielded ages different than expected from the archaeological context.
The AixMICADAS facility is in part dedicated to research on radiocarbon (14C) calibration by means of various archives. For this purpose, we are improving upon the capacity to accurately date subfossil wood. In the current study, nine chemical pretreatment protocols are tested on six wood samples of known ages. The optimization based on 14C ages, 13C/12C ratios, carbon % and overall mass yield % leads us to favor the acid-base-acid-bleaching pretreatment (ABA-B). This efficient method is shown to provide a residue of holocellulose with optimal blanks equivalent to an age of 51,300 14C BP with a standard deviation of 1500 yr based on 25 analyses. The seven wood samples from the Sixth International Radiocarbon Intercomparison (SIRI) are then analyzed as a further verification of the accuracy of our method. As a first scientific contribution, we studied two tree-ring sequences from subfossil pines (Barb12 and Barb17) collected in the southern French Alps. New 14C analyses were performed at high resolution (every third year) and are shown to agree well with results obtained previously by high precision β-counting on CO2 from large samples at lower resolution for Barb17 and accelerator mass spectrometry (AMS) data for Barb12. The new 14C series are then matched to the Kauri and YDB chronologies: the new sequence of Barb12-17 tentatively corresponds to the interval between 12,836 and 12,594 cal BP within the Younger Dryas cold period. The 14C comparison between the Barb12-17 sequence from France and the Kauri sequence from New Zealand allows calculating the 14C Inter-Hemispheric Gradient (IHG), with an average value of ca. 57 yr. The IHG stayed relatively high throughout the studied period. Interestingly, the IHG exhibits a transient maximum value (ca. 100 yr) during the period of rapid Δ14C rise (12,750–12,720 cal BP), a behavior that could be due to a delayed response of the Southern Hemisphere.
The Ansanto Valley (southern Italy) is characterized by vents and boiling mud lakes that emit typical volcanic exhalations (mostly fossil CO2). This fossil dilution spreads over the Ansanto Valley and its impact on local trees is investigated in this study. Six trees at increasing distance from the emitting sources and 2 aliquots of gas were sampled. Dendrochronological analysis was performed on tree cores in order to check the accuracy of the tree-ring sequences; the results indicate no anomalies in the curves of the analyzed trees. δ13C and radiocarbon (14C) analyses were performed on the α-cellulose extracted from some selected tree rings. The main aim of δ13C analysis was to gain information about the origin of CO2 arising from the source; the results support the hypothesis of a carbonatic origin, with respect to a volcanic origin. 14C analysis was performed to evaluate the influence and to quantify the percentage of fossil dilution characterizing the local atmosphere and affecting the trees at different distances from the source during the years. The results show the presence of a strong fossil dilution affecting the trees, increasing toward the sources (from ∼6% at 80 m distance to ∼30% at 20 m from the nearest vent) with quite stable values over the examined period.
Nine excavation seasons at Ossimo Anvòia in the Val Camonica (Central Alps, Italy) have brought to light a Copper Age ceremonial area with symbolic monoliths (statue menhirs) in their original position. Hundreds of artifacts and ecofacts indicate ideological activity during the 3rd millennium BC. A large pit (F18) was discovered that was unusual for its great size and the abundance of well-preserved charcoal. The pit housed a fallen monolith (M9) showing complicated reshaping. A detailed spatial study based on 6 radiocarbon accelerator mass spectrometry (AMS) measurements combined with charcoal analysis has untangled key information to define the history of feature F18-M9. 14C data show that the burning event occurred most probably in the 4th century AD, not in prehistory. We infer a unique episode of “reconsecration” during the very latest phases of pagan cult activity in the Val Camonica. Further studies are needed to resolve the relationships with other features of the site. In addition, charcoal analysis has produced paleobotanical information for a scarcely known period in the environmental history of the area. A sparse forest with Picea abies, Larix decidua, and Fagus sylvatica existed, associated with areas likely devoted to grazing. There is a remarkable absence of chestnut.
This paper reports the results from applying the Cryo2SoniC (Cryobreaking, Sonication, Centrifugation) protocol to some lime mortars sampled from the citadel of Shayzar (Syria). The overall aims of this project are 1) to use the properties offered by high-precision accelerator mass spectrometry (AMS) radiocarbon dating for the evaluation of absolute chronology with its typical robust time constraints (i.e. 25 14C yr), and 2) to apply the dating directly to the citadel structures in order to prevent possible biasing effects potentially affecting indirect 14C dating on organic materials found at the study site. The analyses presented in this paper have been mainly performed as a preliminary check of the Cryo2SoniC methodology in order to assess its applicability to this study site by comparing observed mortar results with archaeological expectations about the citadel development phasing and charcoals found encased in mortars. Petrographic and mineralogical thin-section analyses by optical microscopy (TSOM), X-ray powder diffraction (XRD), and scanning electron microscopy plus energy dispersive spectroscopy (SEM/EDS) investigations were carried out for characterization of the mortar samples to verify the occurrence of some features, related to their production technology, which may introduce dating offsets. The resulting 14C calibrated ages were in agreement with the archaeological expectations based on type and stratigraphic site reconstructions, in situ inscriptions, and written sources. Such results showed also a general (with 1 exception) statistical agreement among the charcoals and the analyzed mortars simultaneously, confirming the archaeological expectations for the Shayzar citadel. Results presented in this paper indicate good accuracy for the applied procedure for chronology reconstruction and highlight the capability of Cryo2SoniC to further characterize the Shayzar site.
Bone chemical treatment for radiocarbon dating has drawn the attention of different laboratories because dates of bones and charcoals found in the same layer often disagree. Excluding diet-related reservoir effects, this observation is likely due to a nonoptimized procedure of contaminant removal from the extracted collagen. In this study, systematic work on the bone chemical treatment was performed with the aim to investigate the effect of each known procedure (i.e. AAA, GEL, and ULTR) on the collagen used for 14C dating. Isolation and purification of lipids from animal tissues were performed to estimate eventual offsets induced by the applied methods, by comparing the 14C ages of lipids with those of collagen. Moreover, cremated bones were treated for the first time at CIRCE. Measured 14C isotopic ratios on these samples were used to evaluate the accuracy of the applied procedure by comparing against the results for charcoals found in the same archaeological context as the bones.
The Ansanto Valley (southern Italy) is characterized by hydrothermal phenomena, with volcanic gas emissions arising from some vents. In the 1 st millennium BC, a sanctuary dedicated to the goddess Mephitis was built but later destroyed by landslides in the valley. During archaeological excavations in the 1950s, many items were found including wooden artifacts, preserved thanks to the imbibition and subsequent mineralization of the wood tissues due to the gas emissions. Radiocarbon dating of these objects is underway at CIRCE (Centre for Isotopic Research on Cultural and Environmental Heritage), in Caserta, Italy. Unfortunately, 2 main problems arise in dating these materials. The first is possible fossil dilution caused by the CO2 emitted from the nearby volcanic vents, which could affect the trees of the valley and also the archaeological materials. In order to determine the magnitude of the fossil dilution in the area, 14C measurements were performed on contemporaneous wood cored from 2 oak trees growing near the vents. 14C values measured in these samples confirmed the presence of a strong fossil dilution in the Ansanto Valley. The second problem is the restoration that the objects underwent during the last century (mostly by using modern organic substances). To investigate suitable pretreatment procedures for removing the restoration materials from the archaeological findings, contemporaneous wood was also analyzed. The wood of trees from the Ansanto Valley and from a distant village (unaffected by the Ansanto fossil dilution) were submitted to the same restoration process applied to the archaeological artifacts, followed by an “artificial weathering” process. Some archaeological materials were also tested for the removal of restoration materials. We subjected the artificially aged trees and the archaeological samples to different chemical processes. Here, we present the results of these processes. Almost all methods turned out to be suitable for the contemporaneous wood, while the results for the archaeological samples remain uncertain. For this reason, more tests are needed, concerning the “artificial weathering,” the restoration, and the chemical procedure for removing the consolidation materials.
An ancient pottery workshop belonging to the Han Dynasty was excavated in Caoxie village, Hepu County. Caoxie village is an important archaeological site in Hepu County, Beihai City, in south China's Guangxi Zhuang Autonomous Region. It is believed that Hepu County was the oldest departure point on the ancient maritime trading route during the Han Dynasty (206 BC to AD 220) due to the ideal natural geographical conditions and the existence of a large number of Han tombs. Radiocarbon measurements on wood and charcoal samples from the Caoxie village site were performed at the Peking University AMS facility (PKU-AMS), Beijing, and the Centre for Isotopic Research for Cultural and Environmental Heritage (CIRCE) at Naples Second University, Italy. Calibrated ages were obtained with code CALIB 5 (Stuiver and Reimer 1993). The results of these measurements are presented and the related chronology is discussed.
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