In this study, we investigate quartz-based luminescence optical dating of Iron Age deposits at the archaeological site of Tell Damiyah in the Jordan valley. Ten samples, taken from different occupation layers from two different excavation areas, proved to have good luminescence characteristics (fast-component dominated, dose recovery ratio 1.032 ± 0.010, n=24). The optical ages are completely consistent with both available 14C ages and ages based on stylistic elements; it appears that this material was fully reset at deposition, although it is recognised that the agreement with age control is somewhat dependent on the assumed field water content of the samples. Further comparison with different OSL signals from feldspar, or investigations based on dose distributions from individual grains would be desirable to independently confirm the resetting of this material. It is concluded that the sediments of Tell Damiyah are very suitable for luminescence dating. Despite the relatively large associated age uncertainties of between 5 and 10%, OSL at tell sites has the potential to provide ages for material very difficult to date by conventional methods, and to identify reworked mixtures of older artifacts in a younger depositional setting.

The most recent workshop on mortar dating (25–27 Oct. 2018, Bordeaux, Montaigne University, France), which closely followed the publication of an extensive round robin-exercise involving several laboratories, was an opportunity to review the history and challenges of mortar dating methods and procedures currently in use. This review stems from the keynote lectures presented at the meeting, and wishes to summarize recent results, present trends, and future challenges. Three major areas are brought into focus (1) radiocarbon (14C) dating of complex mortars: can we assess the chances of successful dating?, (2) 14C dating of archaeological carbonate materials: difficulties, new directions and applications, and (3) single grain optically stimulated luminescence (OSL) dating of mortars in architectural archaeology: the current state of the art. This paper reflects the material presented by the authors and discussed at the workshop.

Given the nature of medieval artifacts and resulting research requirements, a precise temporal classification is essential. It is especially important for the purposes of medieval archaeology in interpreting archaeological finds/finding situations and identifying them with a historical events or figures, for example, to identify skeletal remains of a known historical figure or to establish a chronological sequence of various cultural and architectural changes within an area. Due to the fact that the uncertainties of radiocarbon (14C) analyses have been decreasing in recent years, the applicability of 14C dating for such purposes is now growing. In this work, we aim to demonstrate the current possibilities of the use of AMS 14C analyses on specific cases and confront the results with other available data. 14C data from skeletal remains of members of the oldest Czech ruling dynasty of the Přemyslids (about 880–1306 AD) were obtained in recent years. Archaeological research conducted in the three oldest churches in the Prague Castle discovered skeletal remains of three members of the second, two members of the fourth and two members of the fifth generation. This case study of the application of 14C data has three parts: i) identification of excavated individuals; ii) demonstration of the application using current AMS-based analysis of 14C on medieval osteological material and tests of our preparation method; iii) contributing to discussion and consulting with other problematical 14C age alteration influenced by diet, age of bone collagen or seasonal variation of 14C activity. The obtained results and the issues arising from them clearly highlight the necessity of a multidisciplinary cooperation in this type of study.

The otoliths (ear stones) of fishes are commonly used to describe the age and growth of marine and freshwater fishes. These non-skeletal structures are fortuitous in their utility by being composed of mostly inorganic carbonate that is inert through the life of the fish. This conserved record functions like an environmental chronometer and bomb-produced radiocarbon (14C)—a 14C signal created by atmospheric testing of thermonuclear devices—can be used as a time-specific marker in validating fish age. However, complications from the hydrogeology of nearshore marine environments can complicate 14C levels, as was the case with gray snapper (Lutjanus griseus) along the Gulf of Mexico coast of Florida. Radiocarbon of these nearshore waters is influenced by freshwater input from the karst topography of the Upper Floridan Aquifer—estuarine waters that are 14C-depleted from surface and groundwater inputs. Some gray snapper likely recruited to this kind of environment where 14C levels were depleted in the earliest otolith growth, although age was validated for individuals that were not exposed to 14C-depleted waters to an age of at least 25 years with support for a 30-year lifespan.

A new method to extract CO2 in seawater samples for the determination of F14C has been developed in the Laboratory of Ion Beam Physics at ETH Zurich. The setup consists of an automated sampler designed to extract dissolved inorganic carbon (DIC) from 7 samples in a row, by flushing the seawater with He gas to extract CO2. The fully automated method is controlled via a LabVIEW program that runs through all consecutive steps: catalyst preconditioning, CO2 extraction, CO2 trapping, thermal CO2 release from the trap into the reactor and finally the graphitization reaction which is performed simultaneously in the 7 reactors. The method was optimized by introducing a Cu-Ag furnace that was placed between the water and zeolite traps, which resulted in a better and faster graphitization performance (<2 hr) compared to previously used techniques. The method showed to be reproducible with an unprecedented precision of 1.7‰ even though consuming only 50–60 mL of seawater. The high throughput of 21 samples per day allows for coverage of future oceanographic transects with high spatial resolution, thus fostering the use of radiocarbon (14C) as water mass tracer.

As part of the study of the early medieval cemetery at Broechem (Belgium), human bones from 32 cremation graves have been dated through radiocarbon (14C) analysis. It was noted that many of the dates were not in accordance with the chronological ranges provided by the characteristics of the cultural artifacts deposited in the graves. In fact, the human bones were “older” than the artifacts. Subsequently, a number of animal bones (in all cases from domestic pigs) was radiocarbon dated, yielding dates that were more consistent with the information from the cultural artifacts than the human bones. The dates obtained on human and pig bones from the same grave often differed around 100 radiocarbon years. This paper tries to find an explanation for the pattern observed, concentrating on two hypotheses: aquatic reservoir versus old wood effects. The evaluation takes into account additional radiocarbon dates derived from charcoal fragments of the funeral pyre, from both short-lived and long-lived taxa. A conclusive explanation for the anomalous radiocarbon dates could not be reached but clear suggestions can be put forward for future experimental work that will without doubt shed more light upon the interpretational problems raised.

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.

The formation of commingled human bone assemblages is a key aspect for better understanding funerary rituals. The megalithic cemetery of Panoría (Spain) provides an excellent opportunity to explore bone assemblage formation thanks to the recent excavation of an undisturbed burial. For this purpose, we have approached the differential skeletal representation found between bone and teeth at the site through radiocarbon (14C) dating and Bayesian modeling. The comparison between the series of 14C dates on bone (n=12) and teeth (n=14) stress three main aspects: (1) the dates of teeth show a long period of funerary use before the deposition of the human bone remains; (2) both kinds of samples appear to be chronologically sequenced; the end of the teeth 14C series matches with the beginning of human bone deposition; and (3) bone remains span a short period, not more than a few decades, which probably represents the last episode of intense mortuary activity. These differences suggest that teeth could be the evidence of skeletal depositions subsequently removed from the tomb. The deposition and removal of bone remains emerge as key aspects in the formation of the bone assemblage.

Early researchers of radiocarbon levels in Southern Hemisphere tree rings identified a variable North-South hemispheric offset, necessitating construction of a separate radiocarbon calibration curve for the South. We present here SHCal20, a revised calibration curve from 0–55,000 cal BP, based upon SHCal13 and fortified by the addition of 14 new tree-ring data sets in the 2140–0, 3520–3453, 3608–3590 and 13,140–11,375 cal BP time intervals. We detail the statistical approaches used for curve construction and present recommendations for the use of the Northern Hemisphere curve (IntCal20), the Southern Hemisphere curve (SHCal20) and suggest where application of an equal mixture of the curves might be more appropriate. Using our Bayesian spline with errors-in-variables methodology, and based upon a comparison of Southern Hemisphere tree-ring data compared with contemporaneous Northern Hemisphere data, we estimate the mean Southern Hemisphere offset to be 36 ± 27 14C yrs older.

After the sharp transition to aridity that followed the “Green Sahara” episode 5500 years ago, human settlements took refuge in Egyptian oases, which have to varying extents been “Green Oases” for centuries. In that period, synchronous with the beginning of historical times, the desert’s aridity is generally regarded as broadly comparable to the current period. Natural and anthropogenic deposits studied during 13 excavation campaigns in Bahariya Oasis (Egyptian Desert) suggest that a fairly clear transition from a relatively green environment to much more arid landscapes occurred in the first millennia BCE and CE. This article aims at establishing the chronology of human occupations and environmental change within this period, by combining archaeological and radiocarbon data, using Bayesian modeling. It reveals that the drying up of the environment experienced by desert farmers occurred at some point between the reigns of Antoninus Pius and Caracalla (2nd–3rd century CE). The accuracy of the produced chronological models made it possible to highlight synchronisms between the end of this “Green Oasis” phase and comparable aridification phenomena on regional and interregional scales. Similar degradation processes on remote sites inside the Roman Empire might be explained by globalized anthropogenic agencies overlapping with a broader climatic drying.

Micropaleontological and geochemical data were applied to sediments from southeastern Brazil to study the hydrodynamics associated with the Holocene sea level rise. Sediment cores were taken around Vitória Bay, examined for dinoflagellate cysts and subjected to isotopic analysis. The cyst assemblage mainly dominated by autotrophic species most notably O. centrocarpum, L. machaerophorum and T. vancampoae. The influence of the marine transgression and subsequent regression observed during the Holocene along the coast of Brazil could have initially favored the establishment of an oligotrophic and higher energy environment. The inflow of continental water from tributaries combined with a higher inflow of saline water into the estuarine system could have favored the establishment and subsequent deposition of the dinocysts.

The Mayan Codex of Mexico (MCM), the only Mayan codex found in the 20th century, was unveiled in 1971 during the Ancient Maya Calligraphy exhibition at Club Grolier. The codex comprises 10 pages of bark paper in accordion format, coated with a layer of plaster on both sides. It illustrates the synodic cycles of Venus, with its four phases. Since its discovery, the MCM has been subject to controversy and discussions about its authenticity. In 2016, a group of specialists led by Baltazar Brito chief of the National Library of Anthropology and History, carried out an exhaustive study of the codex with the purpose of determining its temporality and authenticity. In this work, the pre-Columbian authenticity of the codex is verified by the radiocarbon (14C) technique using AMS. Two cleaning procedures were contrasted: the standard acid-base-acid (ABA) protocol and a second one with Soxhlet plus ABA. Results obtained when samples were prepared following ABA protocol only, placed the age of the bark paper between 991 and 1147 cal AD. The second cleaning method with Soxhlet plus ABA, resulted in younger ages, between 1159 and 1261 cal AD. However, we consider that when Sohxlet is used as part of the cleaning protocol, organic contaminants are reduced to a minimum, and 14C dates are more reliable. These results indicate that the vegetal support of the MCM belongs to Postclassical Mayan period and place it as the oldest known manuscript of America found to date.

Hydraulic lime binders are considered a technological marvel which revolutionized construction techniques in antiquity. The core material is made of a binder that is a mixture of calcite and hydraulic phases, which are amorphous silicate compounds that nanostructurally polymerize into insoluble phases that harden even underwater, formed during the reaction between lime and reactive silicates such as volcanic ash. This is also what makes hydraulic lime so hard to radiocarbon (14C) date. These insoluble phases contain carbonates that may set centuries following their application, resulting in younger ages, which may contaminate the calcite fraction that is favorable for 14C dating. This calcite fraction forms upon the incorporation of atmospheric carbon dioxide during the setting of the hydrated lime. Therefore, different characterization methods are being constantly developed for identifying and characterizing the components of hydraulic lime-binders. In this work, we present a rapid characterization technique based on Fourier transform infrared spectroscopy (FTIR) that characterizes the atomic disorder and chemical environment of the carbonates and silicates fractions in the binder. The atomic disorder of the calcite crystallites was determined by the ν2 and ν4 vibrational modes, and the silicates were characterized by the main peak asymmetry and full width at half maximum (FWHM). Different hydraulic binders from Caesarea Maritima were examined, including Herodian mortars from the underwater breakwater and on-land plasters and mortars from the portʼs warehouse and vaults. Hydraulic binders, in which the calcite fraction in the binder shows atomic disorder that is comparable to modern plaster binders, was associated with silicates that have asymmetry and FWHM of clays and quartz. These materials are considered to be in good preservation state for 14C dating since their carbonates crystallites are disordered and did not interact with the environment chemically to form stable and ordered crystals. Interestingly, the atomic disorder of binders that underwent chemical alterations and recrystallization processes, are associated with reactive silicates aggregates such as volcanic ash (pozzolana). These results suggest a new way to prescreen materials for radiocarbon dating based on the composition of lime-binders and preservation state of the carbonate fraction and hydraulic products.

Accurate radiocarbon (14C) dating of lime mortars requires a thorough mineralogical characterization of binders in order to verify the presence of carbon-bearing contaminants. In the last 20 years, cathodoluminescence (CL) has been widely used for the identification of geologic calcium carbonate (CaCO3) aggregates and unreacted lime lumps within the particle size fraction selected for carbon recovery. These components are major sources of older and younger carbon, respectively, and should be removed to obtain accurate age determinations. More recently, laser-induced fluorescence (LIF) has provided another means of investigating the preservation state and composition of CaCO3 binders. Considered the growing interest of the mortar dating community in the latest advancements of these analytical methods, here we review the principles of CL and LIF of CaCO3, their instrument setup, and their application to the characterization of ancient lime mortars used for 14C dating. In addition, we provide examples of SEM-CL and LIF analyses using high-resolution instrumentation, we discuss current issues and propose future lines of research.

The direct dating of rock paintings is not always possible due to the lack of organic carbon compounds in pigments, or because sampling from a heritage site is often restricted. To overcome these limitations, dating laboratories have to develop new approaches. In this study, we consider sampling calcium oxalate crusts covering the painted artworks as a way to indirectly date the rock art. This stratigraphic approach includes isolating and extracting pure oxalate from the crusts. The approach was tested on natural bulk accretions collected in the open-air sites of Erongo Mountains in Namibia. The accretions were separated into two phases (pure oxalate and the remaining residues) with a special pretreatment. This process removes carbonates through acidification (HCl 6N) and dissolves the oxalate into the supernatant, leaving the minerals and windblown organic compounds in the residue. The efficiency of the separation was checked on the two phases by FTIR analyses and by 14C dating and showed that pure oxalate powders were indeed obtained. AMS radiocarbon results of various accretions on the same art panels provided ages from modern periods to 2410 ± 35 BP. From these first results, more targeted sampling campaigns can be considered to provide a terminus ante quem for the rock art.