Human response to the Younger Dryas along the southern North Sea basin, Northwest Europe.

Currently in NW Europe little is known about the human response to the extensive cold reversal at the end of the Pleistocene, the Younger Dryas (ca. 12,850 till ca. 11,650 cal BP), mainly due to the poor chronological resolution of the archaeological sites belonging to the Ahrensburgian Culture. Here we present a series of 33 radiocarbon dates performed on the seminal cave site of Remouchamps, situated in the Belgian Meuse basin. Combined with a revision of the available radiocarbon evidence along the southern North Sea basin (Belgium, southern Netherlands, western Germany), it is suggested that the first half of the Younger Dryas, characterized as extremely cold and wet, faced a significant population reduction. Repopulation started around the middle of the Younger Dryas, from ca. 12,200 cal BP onward, probably in response to a slight climatic improvement leading to somewhat warmer summers. This might be considered a prelude to the subsequent population boost of the Early Holocene (Mesolithic).

A new multi-analytical procedure for radiocarbon dating of historical mortars.

The overarching challenge of this research is setting up a procedure to select the most appropriate fraction from complex, heterogeneous materials such as historic mortars in case of radiocarbon dating. At present, in the international community, there is not a unique and fully accepted way of mortar sample preparation to systematically obtain accurate results. With this contribution, we propose a strategy for selecting suitable mortar samples for radiocarbon dating of anthropogenic calcite in binder or lump. A four-step procedure is proposed: (I) good sampling strategies along with architectural and historical surveys; (II) mineralogical, petrographic, and chemical characterization of mortars to evaluate the feasibility of sample dating; (III) a non-destructive multi-analytical characterization of binder-rich portions to avoid geogenic calcite contamination; (IV) carbonate micro-sample preparation and accelerator mass spectrometer (AMS) measurements. The most innovative feature of the overall procedure relies on the fact that, in case of positive validation in step III, exactly the same material is treated and measured in step IV. The paper aims to apply this procedure to the ancient mortar of the Florentine historical building (Trebbio Castle), selecting micro-samples suitable for dating in natural hydraulic mortars. The discussion of the mortar dating results with the historical-archaeological hypotheses provided significant insights into the construction history of the building.

Demystifying the tropics: FTIR characterization of pantropical woods and their α-cellulose extracts for past atmospheric 14C reconstructions.

To ensure unbiased tree-ring radiocarbon (14C) results, traditional pretreatments carefully isolate wood cellulose from extractives using organic solvents, among other chemicals. The addition of solvents is laborious, time-consuming, and can increase the risk of carbon contamination. Tropical woods show a high diversity in wood-anatomical and extractive composition, but the necessity of organic-solvent extraction for the 14C dating of these diverse woods remains untested. We applied a chemical treatment that excludes the solvent step on the wood of 8 tropical tree species sampled in South-America and Africa, with different wood-anatomical and extractive properties. We analyzed the success of the extractive removal along with several steps of the α-cellulose extraction procedure using Fourier Transform Infrared (FTIR) spectroscopy and further confirmed the quality of 14C measurements after extraction. The α-cellulose extracts obtained here showed FTIR-spectra free of signals from various extractives and the 14C results on these samples showed reliable results. The chemical method evaluated reduces the technical complexity required to prepare α-cellulose samples for 14C dating, and therefore can bolster global atmospheric 14C applications, especially in the tropics.

Radiocarbon chronology of Iron Age Jerusalem reveals calibration offsets and architectural developments.

Reconstructing the absolute chronology of Jerusalem during the time it served as the Judahite Kingdom's capital is challenging due to its dense, still inhabited urban nature and the plateau shape of the radiocarbon calibration curve during part of this period. We present 103 radiocarbon dates from reliable archaeological contexts in five excavation areas of Iron Age Jerusalem, which tie between archaeology and biblical history. We exploit Jerusalem's rich past, including textual evidence and vast archaeological remains, to overcome difficult problems in radiocarbon dating, including establishing a detailed chronology within the long-calibrated ranges of the Hallstatt Plateau and recognizing short-lived regional offsets in atmospheric 14C concentrations. The key to resolving these problems is to apply stringent field methodologies using microarchaeological methods, leading to densely radiocarbon-dated stratigraphic sequences. Using these sequences, we identify regional offsets in atmospheric 14C concentrations c. 720 BC, and in the historically secure stratigraphic horizon of the Babylonian destruction in 586 BC. The latter is verified by 100 single-ring measurements between 624 to 572 BC. This application of intense 14C dating sheds light on the reconstruction of Jerusalem in the Iron Age. It provides evidence for settlement in the 12th to 10th centuries BC and that westward expansion had already begun by the 9th century BC, with extensive architectural projects undertaken throughout the city in this period. This was followed by significant damage and rejuvenation of the city subsequent to the mid-eight century BC earthquake, after which the city was heavily fortified and continued to flourish until the Babylonian destruction.

An archaeobotanical and stable isotope approach to changing agricultural practices in the NW Mediterranean region around 4000 BC.

It has recently been observed, that a change in the crop spectrum happened during the so-called Middle Neolithic in France at ca. 4000 BC. An agricultural system based on free-threshing cereals (naked wheat and naked barley) seems to shift to one based on glume wheats. This is a major change for traditional farmers and this paper aims to shed light on its possible causes. Here we describe the results of new investigations in a key area for the understanding of this process: the NW Mediterranean arch, where free-threshing cereals are the main cultivars since ca. 5100 BC. New data confirm that the shift towards glume wheats is also observed in some sites of the NE of the Iberian Peninsula and that among the glume wheats that spread at ca. 4000 BC we should not only consider emmer and einkorn but also Timopheevi's wheat. Stable isotope analyses indicate no major decrease in soil fertility or alterations in local precipitation regimes. The agricultural change may be the result of a combination of the spread of damaging pests for free-threshing cereals and presumably new networks being developed with the North-eastern part of Italy and the Balkans.

Neuroanatomy and pneumaticity of the extinct Malagasy "horned" crocodile Voay robustus and its implications for crocodylid phylogeny and palaeoecology.

Voay robustus, the extinct Malagasy "horned" crocodile, was originally considered to be the only crocodylian representative in Madagascar during most part of the Holocene. However, Malagasy crocodylian remains have had confused taxonomic attributions and recent studies have underlined that Crocodylus and Voay populations coexisted on the island for at least 7500 years. Here, we describe the inner braincase anatomy of Voay robustus using x-ray computed tomography on four specimens, to provide new anatomical information that distinguishes Voay from Crocodylus, especially features of the brain endocast and the paratympanic sinuses. Geometric morphometric analyses are performed on 3D models of the internal organs to compare statistically Voay with a subset of extant Crocodylidae. Following these comparisons, we build an endocranial morphological matrix to discuss the proposed phylogenetic affinities of Voay with Osteolaeminae from an endocranial point of view. Additionally, we discuss the use of internal characters in systematic studies and find that they can have a major impact on morphological analyses. Finally, new radiocarbon data on Voay and subfossil Crocodylus specimens are recovered between 2010 and 2750 cal BP, which confirm the cohabitation of the two species in the same area for a long period of time. We thus assess several extinction scenarios, and propose a slightly different ecology of Voay compared to Crocodylus, which could have allowed habitat partitioning on the island. Our approach complements information obtained from previous molecular and morphological phylogenies, as well as previous radiocarbon dating, together revealing past diversity and faunal turnovers in Madagascar.

The name of the game: palaeoproteomics and radiocarbon dates further refine the presence and dispersal of caprines in eastern and southern Africa.

We report the first large-scale palaeoproteomics research on eastern and southern African zooarchaeological samples, thereby refining our understanding of early caprine (sheep and goat) pastoralism in Africa. Assessing caprine introductions is a complicated task because of their skeletal similarity to endemic wild bovid species and the sparse and fragmentary state of relevant archaeological remains. Palaeoproteomics has previously proved effective in clarifying species attributions in African zooarchaeological materials, but few comparative protein sequences of wild bovid species have been available. Using newly generated type I collagen sequences for wild species, as well as previously published sequences, we assess species attributions for elements originally identified as caprine or 'unidentifiable bovid' from 17 eastern and southern African sites that span seven millennia. We identified over 70% of the archaeological remains and the direct radiocarbon dating of domesticate specimens allows refinement of the chronology of caprine presence in both African regions. These results thus confirm earlier occurrences in eastern Africa and the systematic association of domesticated caprines with wild bovids at all archaeological sites. The combined biomolecular approach highlights repeatability and accuracy of the methods for conclusive contribution in species attribution of archaeological remains in dry African environments.

Large-scale application of palaeoproteomics (Zooarchaeology by Mass Spectrometry; ZooMS) in two Palaeolithic faunal assemblages from China.

The application of Zooarchaeology by Mass Spectrometry (ZooMS) on Pleistocene sites in Europe and northern Asia has resulted in the discovery of important new hominin fossils and has expanded the range of identified fauna. However, no systematic, large-scale application of ZooMS on Palaeolithic sites in East Asia has been attempted thus far. Here, we analyse 866 morphologically non-diagnostic bones from Jinsitai Cave in northeast China and Yumidong Cave in South China, from archaeological horizons dating to 150-10 ka BP. Bones from both sites revealed a high degree of collagen preservation and potentially time-related deamidation patterns, despite being located in very distinct environmental settings. At Jinsitai, we identified 31 camel bones, five of which were radiocarbon dated to 37-20 ka BP. All dated specimens correspond to colder periods of Marine Isotope Stages 3 and 2. We regard the presence of camels at Jinsitai as evidence of wild camels being a megafauna taxon targeted, most likely by early modern humans, during their expansion across northeast Asia. This large-scale application of ZooMS in China highlights the potential of the method for furthering our knowledge of the palaeoanthropological and zooarchaeological records of East Asia.

The histology and growth rate of Nile crocodile (Crocodylus niloticus) claws.

The histology and growth of reptilian and crocodilian claws (ungues) have been extensively studied; however, Nile crocodile (Crocodylus niloticus) claws have not received adequate attention. Furthermore, age estimations for reptilian claws remain unexplored, despite Nile crocodile claws being used in long-term dietary reconstruction studies, assuming certain age-related patterns. In this study, we investigate the histology and growth patterns of Nile crocodile claws, aiming to infer axes for sampling cornified material for radiocarbon dating and establish age estimations for crocodilian claws. Our findings reveal that Nile crocodile claws exhibit growth patterns similar to other reptilians, presenting as modified scutes/scales with an age profile along the sagittal plane. This profile starts at the basal germ matrix and progressively expands in thickness and age dorsoventrally towards the apex or "tip." Consequently, the oldest corneous material is concentrated at the most dorsal point of the claw's apex. To validate previous dietary reconstruction assumptions, we conducted radiocarbon dating on this region of the claw, which supported the idea that retained corneous material in the claws is typically relatively young (5-10 years old) due to abrasion. Our study contributes insights into the histology and growth dynamics of Nile crocodile claws, shedding light on their use in dietary reconstruction studies and emphasizing the significance of considering age-related assumptions in such investigations.

Radiocarbon dating as tool to assist in triaging cases of unidentified human remains in Victoria, Australia: A case series.

In cases where human remains are unidentified because there is no initial identification hypothesis, limited contextual information, and/or poor preservation, radiocarbon (14 C) dating may be a useful tool to further assist with identification. Through measuring the amount of 14 C remaining in organic material, such as bone, teeth, nail, or hair, radiocarbon dating may provide an estimated year of birth and year of death for a deceased person. This information, may assist in, establishing whether a case of unidentified human remains (UHR) is actually of medicolegal significance and therefore, requires forensic investigation and identification. This case series highlights the application of 14 C dating to seven of the 132 UHR cases in Victoria, Australia. Cortical bone was sampled from each case and the level of 14 C was measured to provide an estimated year of death. Four of the seven cases analyzed contained the levels of 14 C consistent with an archeological timeframe, one contained a level of 14 C consistent with a modern (i.e., of medicolegal significance) timeframe, and the results for the remaining two samples were inconclusive. Applying this technique not only reduced the number of UHR cases in Victoria but also has investigative, cultural, and practical implications for medicolegal casework in general.

Status report of the first AMS laboratory in the Czech Republic at the Nuclear Physics Institute, Rez.

The first accelerator mass spectrometry (AMS) laboratory in the Czech Republic has been established and put into routine operation in February 2022. Here we briefly describe the facilities available, namely a 300 kV multi-isotope low-energy AMS system (MILEA) capable of determination 10Be, 14C, 26Al, 41Ca, 129I, isotopes of U, especially 236U, Pu and other actinoids, and accessories for 14C measurements, which include a gas interface system, a preparative gas chromatography system for compound-specific radiocarbon dating analysis, and an isotope-ratio mass spectrometer. The first results achieved for separation and measurement of the above radionuclides (except for 41Ca) are also reported, with the main focus on 14C measurements. A specimen breakdown of 729 graphitised samples analysed for 14C so far is presented, as well as a proof of measurement stability of the MILEA system obtained by analysis of radiocarbon standards and analytical blanks. For the other radionuclides, well proven or novel procedures for sample preparation and measurement are presented.

The effects of diet and beauty products on the uptake and storage of 14C in hair and nails: ramifications for the application of bomb pulse dating to forensic anthropological casework.

Radiocarbon dating is a useful tool in the examination of unknown human remains. Recent studies have shown that the analysis of hair and nail samples can provide a highly accurate estimation of the year of death (YOD). However, little research has examined factors that may influence the uptake and storage of 14C in these tissues, such as diet, or the use of beauty products. This study measured the level of 14C in human hair and nail samples collected from living individuals to determine whether diet, and the use of hair dye or nail polish, has a significant impact on the estimation of YOD. The results of this study showed that diet did not appear to impact the radiocarbon content in human hair and nail, and thus should not be considered a limitation when analysing samples obtained from unidentified human remains. The use of nail polish, and in the majority of cases, hair dye, did not significantly impact the 14C concentration in nails and hair. While the results of this study are preliminary, they suggest that in most cases, both hair and nail can be successfully analysed using radiocarbon dating to estimate an individual's YOD. However, best practice should involve the analysis of multiple tissue types, to minimise any error that may be introduced as a result of the decedent's use of beauty products.

Addressing forensic science challenges with nuclear analytical techniques - A review.

We review the application of Nuclear Analytical Techniques (NATs) to forensic problems for the first time. NATs include neutron activation analysis (NAA), carried out in nuclear reactors for elemental analysis; accelerator-based techniques, mainly Ion Beam Analysis (IBA) for elemental and molecular analysis; and Accelerator Mass Spectrometry (AMS) for dating of traces of forensic interest by "radiocarbon dating" and other related methods. Applications include analysis of drugs of abuse, food fraud, counterfeit medicine, gunshot residue, glass fragments, forgery of art objects and documents, and human material. In some applications only the NATs are able to provide relevant information for forensic purposes. This review not only includes a wide collection of forensic applications, but also illustrates the wide availability worldwide of NATs, opening up opportunities for an increased use of NATs in routine forensic casework.

On the traces of lost identities: chronological, anthropological and taphonomic analyses of the Late Neolithic/Early Eneolithic fragmented and commingled human remains from the Farneto rock shelter (Bologna, northern Italy).

The present study examines the prehistoric human skeletal remains retrieved starting from the 1920s in the deposit of the Farneto rock shelter, situated in the area of the 'Parco dei Gessi Bolognesi e Calanchi dell'Abbadessa' (San Lazzaro di Savena, Bologna, northern Italy). An exact dating and a reliable interpretation of the assemblage had not been reached so far because of the lack of contextual data useful for dating purposes, the inaccurate recovery procedures of the remains and their state of preservation. In fact, the skeletal remains from the Farneto rock shelter are highly fragmented and commingled, whereas reliable information about their original position and their recovery procedures are not available. Despite these difficulties, radiocarbon analyses allowed the precise dating of the remains to a final phase of the Neolithic and an early phase of the Eneolithic period in Emilia Romagna (northern Italy). The study of the assemblage enabled to clarify the use of the context for funerary purposes. Moreover, the anthropological and taphonomic analyses of the skeletal remains shed light on the biological profile of the individuals and on some events that occurred after their death. In particular, the analysis of perimortem lesions highlighted the existence of intentional interventions related to corpse treatment, referable to dismembering/disarticulation and scarnification, i.e. cleaning of bones from soft tissues. Finally, the comparison with other Italian and European Neo/Eneolithic funerary contexts enabled a better understanding of these complex ritual practices. Supplementary Information: The online version contains supplementary material available at 10.1007/s12520-023-01727-2.

Early Upper Paleolithic cultural variability in the Southern Levant: New evidence from Nahal Rahaf 2 Rockshelter, Judean Desert, Israel.

The Levantine Early Upper Paleolithic (ca. 45-30 ka) has been a focus of research because of its unique position as a conduit of human, flora, and fauna species between Africa and Eurasia. Studies have mainly focused on the Early Ahmarian and Levantine Aurignacian, two entities, the former endemic and the latter foreign, which are considered to have coinhabited the region during that period. However, other cultural entities, such as the Atlitian in the Mediterranean region and the Arkov-Divshon in the arid regions of the southern Levant received less attention, and accordingly, suffer from broad definitions and chronological insecurity. These cultures hold potential insights regarding nuanced adaptations, reciprocal influences, and diachronic assimilation processes. The recently discovered site of Nahal Rahaf 2 Rockshelter in the Judean Desert provides integral information on one of these entities-the Arkov-Divshon. Two excavation seasons revealed a sequence of archaeological layers, with lithic assemblages in which laterally carinated items were prominent. Alongside rich faunal assemblages, other components of the material culture include perforated marine shells and bone tools, marking the first association of these elements with Arkov-Divshon and implying some degree of contact with the Mediterranean regions of the Levant. Good preservation of organic materials allowed radiocarbon dating of the human occupation at the site to ca. 37.5-34.0 ka cal BP, indicating chronological overlap with the Levantine Aurignacian, and possibly also with the latest phases of the Early Ahmarian. Thus, challenging the validity of the widely accepted 'Two Tradition' Model of the Levantine Upper Paleolithic. Lithic analyses suggest the use of one main reduction sequence and the primary production of bladelets from carinated items. Faunal remains suggest targeted hunting of ibex and gazelle. Botanical remains and sedimentary analyses suggest roughly similar environmental conditions, with a possible woodier environment in the surroundings of the site.

Radiocarbon and wood anatomy as complementary tools for generating tree-ring records in Bolivia.

The science of tropical dendrochronology is now emerging in regions where tree-ring dating had previously not been considered possible. Here, we combine wood anatomical microsectioning techniques and radiocarbon analysis to produce the first tree-ring chronology with verified annual periodicity for a new dendrochronological species, Neltuma alba (commonly known as "algarrobo blanco") in the tropical Andes of Bolivia. First, we generated a preliminary chronology composed of six trees using traditional dendrochronological methods (i.e., cross-dating). We then measured the 14C content on nine selected tree rings from two samples and compared them with the Southern Hemisphere (SH) atmospheric 14C curves, covering the period of the bomb 14C peak. We find consistent offsets of 5 and 12 years, respectively, in the calendar dates initially assigned, indicating that several tree rings were missing in the sequence. In order to identify the tree-ring boundaries of the unidentified rings we investigated further by analyzing stem wood microsections to examine anatomical characteristics. These anatomical microsections revealed the presence of very narrow terminal parenchyma defining several tree-ring boundaries within the sapwood, which was not visible in sanded samples under a stereomicroscope. Such newly identified tree rings were consistent with the offsets shown by the radiocarbon analysis and allowed us to correct the calendar dates of the initial chronology. Additional radiocarbon measurements over a new batch of rings of the corrected dated samples resulted in a perfect match between the dendrochronological calendar years and the 14C dating, which is based on good agreement between the tree-ring 14C content and the SH 14C curves. Correlations with prior season precipitation and temperature reveal a strong legacy effect of climate conditions prior to the current Neltuma alba growing season. Overall, our study highlights much potential to complement traditional dendrochronology in tree species with challenging tree-ring boundaries with wood anatomical methods and 14C analyses. Taken together, these approaches confirm that Neltuma alba can be accurately dated and thereby used in climatic and ecological studies in tropical and subtropical South America.

Evaluation of Glycosaminoglycans Biological Age in Cells and Tissues.

Bomb pulse refers to the sharp increase of the atmospheric levels of the carbon isotope 14C due to nuclear testing during the late 1950s and early 1960s. After the nuclear test ban, atmospheric 14C levels decreased exponentially because of the diffusion and equilibration with the ocean and biosphere, as well as the incorporation indirectly into all living cells. Thus, assessing the anthropogenic 14C serves as an isotopic chronometer providing the opportunity to estimate the age of a tissue and its components with a relatively high precision comparing it with the atmospheric levels at a certain time stamp.This protocol describes the use of the bomb pulse dating as a retrospective tracer of tissue components such as the glycosaminoglycans (GAGs) and subsequent proteoglycans turnover using accelerator mass spectrometry.

Suspect graveyard burial (South Armagh, N. Ireland): Combined search, forensic anthropology and radiocarbon dating.

Geophysical investigation of a former convent graveyard for conversion to a community centre identified an unrecorded, unmarked burial below a later burial. Archaeological excavation confirmed the presence of skeletonized human remains, considered by police as a possible clandestine burial. Mortuary examination indicated the remains belonged to a mature adult female. To determine whether the deceased could be a recorded missing person, radiocarbon dating was undertaken on a femur and a rib bone. This is not always straightforward, and results showed two possible ages due to intercepts on either side of the nuclear weapons testing spike in atmospheric 14C; however, the later dated burial allowed us to constrain the date of a rib to CE 1959. This study demonstrates that dating a second tissue with a longer turnaround time, such as a femur, can help to constrain which side of the bomb spike is most probable. This paper documents in one work the search, scene and sample and then advances this to resolution by anthropological analysis and radiocarbon dating of human remains.

Morphological and Tissue Characterization with 3D Reconstruction of a 350-Year-Old Austrian Ardea purpurea Glacier Mummy.

Glaciers are dwindling archives, releasing animal mummies preserved in the ice for centuries due to climate changes. As preservation varies, residual soft tissues may differently expand the biological information content of such mummies. DNA studies have proven the possibility of extracting and analyzing DNA preserved in skeletal residuals and sediments for hundreds or thousands of years. Paleoradiology is the method of choice as a non-destructive tool for analyzing mummies, including micro-computed tomography (micro-CT) and magnetic resonance imaging (MRI). Together with radiocarbon dating, histo-anatomical analyses, and DNA sequencing, these techniques were employed to identify a 350-year-old Austrian Ardea purpurea glacier mummy from the Ötztal Alps. Combining these techniques proved to be a robust methodological concept for collecting inaccessible information regarding the structural organization of the mummy. The variety of methodological approaches resulted in a distinct picture of the morphological patterns of the glacier animal mummy. The BLAST search in GenBank resulted in a 100% and 98.7% match in the cytb gene sequence with two entries of the species Purple heron (Ardea purpurea; Accession number KJ941160.1 and KJ190948.1) and a 98% match with the same species for the 16 s sequence (KJ190948.1), which was confirmed by the anatomic characteristics deduced from micro-CT and MRI.