The aim of the comment is to address the misrepresentations of our work on the Neolithic transitions that are found in a recent article by Manen and coauthors in Radiocarbon. There are a fair number of them as indicated in the comment. The purpose of the comment is (1) to set the record straight, (2) to clarify several misconceptions that have persisted in the literature for some time, and (3) to comment briefly on the convergence between our own recent regional modeling of the spread of early farming along the north coast of the West Mediterranean and the position currently held by Manen and coauthors.

The direct carbonate procedure for accelerator mass spectrometry radiocarbon (AMS 14C) dating of submilligram samples of biogenic carbonate without graphitization is becoming widely used in a variety of studies. We compare the results of 153 paired direct carbonate and standard graphite 14C determinations on single specimens of an assortment of biogenic carbonates. A reduced major axis regression shows a strong relationship between direct carbonate and graphite percent Modern Carbon (pMC) values (m = 0.996; 95% CI [0.991–1.001]). An analysis of differences and a 95% confidence interval on pMC values reveals that there is no significant difference between direct carbonate and graphite pMC values for 76% of analyzed specimens, although variation in direct carbonate pMC is underestimated. The difference between the two methods is typically within 2 pMC, with 61% of direct carbonate pMC measurements being higher than their paired graphite counterpart. Of the 36 specimens that did yield significant differences, all but three missed the 95% significance threshold by 1.2 pMC or less. These results show that direct carbonate 14C dating of biogenic carbonates is a cost-effective and efficient complement to standard graphite 14C dating.

The emergence and widespread distribution of eye fibulae as adornment objects, from the northern provinces of the Roman Empire to northeastern Europe and Scandinavia, as well as their typology have been widely explored. Currently in Lithuania, a total of 209 eye fibulae dating to the 1st and 2nd centuries are known. The geographical distribution, typology and chronology of these Early Roman Period jewelry artifacts do not present any problem. However, the technology of manufacture of these fibulae has been much less studied. The present article analyzes the technology of manufacture of Prussian series eye fibulae, including the previously unknown specific manufacturing techniques, such as the use of wooden axes to modify the construction of the fibula and make it more durable and long lasting. Radiocarbon (14C) dating has unambiguously confirmed that the wooden axes are contemporaneous with the time of the use of the fibulae, while observation under the scanning electron microscope has identified wood species used for making the wooden axes. The X-ray fluorescence spectrometry (XRF) analysis was used to determine the copper alloys, of which eye fibulae were made. The manufacturing technologies of eye fibulae (forging and casting) are discussed in the context of analytical and experimental studies.

The radiocarbon (14C) dating facility at the Centre for Isotope Research, University of Groningen went through a major upgrade in 2017 and this included installation of a MICADAS accelerator mass spectrometer (AMS). In the first 18 months, we performed 4000 sample and 3000 reference measurements. A careful evaluation of those measurement results is presented, to characterize the various sources of uncertainty and to ultimately assign, for every sample measurement, a realistic expanded uncertainty. This analysis was performed on the measurements of secondary references and sample duplicates in various phases of their processing steps. The final expanded uncertainty includes both the 14C measurement uncertainties and uncertainties originating from pretreatment steps. Where the 14C measurement uncertainty includes straightforward uncertainties arising from Poisson statistics, background subtraction, calibration on Oxalic Acid II and δ13C correction, the uncertainties originating from pretreatment steps are based on the spread of actual measurement results for secondary references and sample duplicates. We show that the 14C measurement uncertainty requires expansion, depending on the number of processing steps involved prior to a 14C measurement, by a maximum factor of 1.6 at our laboratory. By using these expansion (multiplication) factors, we make our reported uncertainty both more realistic and reliable.

To elucidate the dynamics of terrestrial leaf waxes in a high-altitude lake system, we performed compound-specific radiocarbon analysis (CSRA) of long-chain n-alkanes in two sediment core sections from Lake Karakul (Pamirs, Tajikistan) and in surface soil samples from the catchment area. We aimed to answer the question whether the n-alkanes are delivered into the lake sediment with substantial delay due to storage in soils, which may cause a potential bias when used as paleoenvironmental proxies. In the surface soils, the CSRA results reveal an age range of n-alkanes from modern to 2278 ± 155 cal BP. In the two sediment core samples, three of the four n-alkane ages fell on the lower ends of the 1σ-uncertainty ranges of modeled ages of the sediments (based on AMS 14C-TOC and OSL dating results). We conclude that sedimentary leaf waxes represent compounds with intermediate turnover time in soils, for example originating from alluvial plains close to the shores. Overall, the results provide evidence that sedimentary leaf wax compounds in this cold and arid setting are potentially older than the conventional age model indicates, but these findings need to be interpreted in context of the generally large uncertainty ranges of such age models.

Here we report radiocarbon measurements made on wheat seed tissue (Triticum aestivum L.; winter or spring type growth habit), from the seed archive of the IPK Gatersleben, Sachsen-Anhalt, Germany, which was harvested between 1946 and 2020. The results give an overview of 75 years of radiocarbon concentration evolution in agricultural plant products. The wheat tissue radiocarbon concentrations follow known pre- and post-bomb radiocarbon records, such as the atmospheric Jungfraujoch, Schauinsland, and NH1 datasets. Based on a Northern Hemisphere growing period from April to July, the Gatersleben seed tissue radiocarbon concentration indicates incorporation of fossil carbon of about 1% with respect to the high alpine, clean-air CO2 of the Jungfraujoch station between 1987 and 2019. We propose to use the pre- and post-bomb radiocarbon record of Gatersleben wheat as a reference in forensic investigations, such as the age estimation of paper by analyzing starch used in paper manufacture. Additionally, an advantage of the record reported here lies in its extensibility by adding new analyses from future harvests.

Dating lime mortar samples using the radiocarbon (14C) method can be difficult. This is because the contamination is similar to the primary dating material (CaCO3) and consequently difficult to remove. Mortar can also have late-in-formation pyrogenic carbonate from interactions with the environment after the initial hardening phase, such as recrystallization, fire damage or delayed hardening. When 14C dating a system of primary dating material, contamination and late-in-formation pyrogenic carbonate, one approach is multi-fraction dating with conclusiveness criteria. If a sample has sufficient contamination or late-in-formation pyrogenic carbonate, the criteria evaluate the result inconclusive. To improve inconclusive results from such samples, this study investigates sample preparation by thermal decomposition. Here samples that were inconclusively dated by the authors’ traditional method, sequential dissolution with 85% phosphoric acid, are investigated further. This study finds that CO2 thermally decomposed at low temperatures contains some late-in-formation pyrogenic carbonate. By rejecting CO2 decomposed at low temperatures, Kastelholm castle and Kimito church in Finland are conclusively and accurately dated. Furthermore, a preheating method removes some late-in-formation carbonate, but not enough for a conclusive result. Finally, thermal decomposition finds difficulty in discerning binder carbonate from limestone and marble contamination.

Manen et al. provide here a reply to the critical comment published by A. J. Ammerman regarding their article “The Neolithic Transition in the Western Mediterranean: a complex and non-linear diffusion process—the radiocarbon record revisited,” published in 2019 in Radiocarbon. They also use this occasion to reaffirm the need to elaborate novel interpretive frameworks that combine both geo-chronological and cultural data.

The last decade has seen the development of a range of new statistical and computational techniques for analysing large collections of radiocarbon (14C) dates, often but not exclusively to make inferences about human population change in the past. Here we introduce rcarbon, an open-source software package for the R statistical computing language which implements many of these techniques and looks to foster transparent future study of their strengths and weaknesses. In this paper, we review the key assumptions, limitations and potentials behind statistical analyses of summed probability distribution of 14C dates, including Monte-Carlo simulation-based tests, permutation tests, and spatial analyses. Supplementary material provides a fully reproducible analysis with further details not covered in the main paper.

Teotihuacan is one of the most studied archaeological sites in Mesoamerica because of its exceptional size and urban planning; however, its last years of occupation and abandonment are still under debate. We report a high-resolution chronology for the Xalla complex integrating archaeomagnetic dates, radiocarbon (14C) ages, and detailed archaeological information about sample type and context in a Bayesian model. The model includes 42 14C ages and 7 archaeomagnetic dates grouped in 6 phases, including samples from collapsed roofs with 14C ages earlier than expected, suggesting a problem of inbuilt age. The archaeomagnetic dates on lime plasters were classified in unburned samples, related to the time of construction, and burned samples, related to the Big Fire associated to the abandonment of Teotihuacan. The modeled 14C ages resulted in shorter intervals, with the possibility of differentiating the construction phases, confirming that big beams had inbuilt age. Further, combining the two dating methods and classifying lime plaster samples in burned and unburned, it was possible to date different events within the same archaeological context. It is concluded that by combining these two dating methods and understanding the moment that each sample is dating, it is possible to obtain solid and precise chronologies.

Coral skeletal structures can provide a robust record of nuclear bomb produced 14C with valuable insight into air-sea exchange processes and water movement with applications to fisheries science. To expand these records in the South Pacific, a coral core from Tutuila Island, American Samoa was dated with density band counting covering a 59-yr period (1953–2012). Seasonal signals in elemental ratios (Sr/Ca and Ba/Ca) and stable carbon (δ13C) values across the coral core corroborated the well-defined annual band structure and highlighted an ocean climate shift from the 1997–1998 El Niño. The American Samoa coral 14C measurements were consistent with other regional records but included some notable differences across the South Pacific Gyre (SPG) at Fiji, Rarotonga, and Easter Island that can be attributed to decadal ocean climate cycles, surface residence times and proximity to the South Equatorial Current. An analysis of the post-peak 14C decline associated with each coral record indicated 14C levels are beginning to merge for the SPG. This observation, coupled with otolith measurements from American Samoa, reinforces the perspective that bomb 14C dating can be performed on fishes and other marine organisms of the region using the post-peak 14C decline to properly inform fisheries management in the South Pacific.

Jacob’s Well, located in modern city of Nablus and ancient Shechem (Tall Balata) in the northern West Bank of Palestine, attracts modern day tourists and pilgrims. It is found in the eastern suburbs of the city. Since 333 AD, pilgrims have been writing accounts of the well, and it has been venerated by both Christian and Jewish communities throughout its history. It is believed to be the well referred to in the New Testament, where Jesus conversed with a Samaritan woman, the orthodox saint, Photini. It now forms the central feature in the crypt of the St Photini Greek Orthodox church in the walled grounds of a monastery. In order to gain more information on the chronology of the site, we analyzed human skeletal remains found at the site in 1997. These consist of three skulls and a femur. One of the skulls was found in a sarcophagus alongside the church and the two other skulls and a femur were found in a burial ground alongside the monastery, north of the church, over which a room has now been built. Radiocarbon analysis reveals that the remains date to four historical periods or events: the early Christian period, before structural additions to the well by Constantine the Great in the fourth century; the Samaritan Revolts (AD 529 and 556), the Sassanid Invasion (AD 614–628), and Abbasid rule (AD 750–1258). Dating of one skull suggests it may have been that of Germanus, a fourth century bishop of Nablus, and that there may have been a very early structure, shrine, or burial chamber at the site before the fourth century. We provide contextual information based on historical and contemporary literature.

The function and change of global soil carbon (C) reserves in natural ecosystems are key regulators of future carbon-climate coupling. Microbes play a critical role in soil carbon cycling and yet there is poor understanding of their roles and C metabolism flexibility in many ecosystems. We wanted to determine whether vegetation type and climate zone influence soil microbial community composition (fungi and bacteria) and carbon resource preference. We used a biomarker (phospholipid fatty acids, PLFAs), natural abundance 13C and 14C probing approach to measure soil microbial composition and C resource use, along a 1900–4167-m elevation gradient on Mount Gongga (7556 m asl), China. Mount Gongga has a vertical mean annual temperature gradient of 1.2–10.1°C and a diversity of typical vegetation zones in the Tibetan Plateau. Soils were sampled at 10 locations along the gradient capturing distinct vegetation types and climate zones from lowland subtropical-forest to alpine-meadow. PLFA results showed that microbial communities were composed of 2.1–51.7% bacteria and 2.0–23.2% fungi across the elevation gradient. Microbial biomass was higher and the ratio of soil fungi to bacteria (F/B) was lower in forest soils compared to meadow soils. δ13C varied between −33‰ to −17‰ with C3 plant carbon sources dominant across the gradient. Soil organic carbon (SOC) turnover did not vary among three soils we measured from three forest types (i.e., evergreen broadleaved subtropical, mixed temperate, coniferous alpine) and dissolved organic carbon (DOC) turnover decreased with soil elevation. Forest soil microbial PLFA 14C and δ13C measurements showed that forest type and climate were related to different microbial C use. The 14C values of microbial PLFAs i15, a15, 16:1, br17 decreased with elevation while those of C16:0, cyC17, and cyC19 did not show much difference among three forest ecosystems. Bacteria and bacillus represented by C16:1 and brC17 showed considerable microbial C metabolism flexibility and tended to use ancient carbon at higher altitudes. Anaerobes represented by cyC17 and cyC19 showed stronger C metabolism selectivity. Our findings reveal specific C source differences between and within soil microbial groups along elevation gradients.

We present two new Bayesian 14C models using IntCal20 that incorporate 17 new calibrated AMS ages for Early Bronze IV Tell Abu en-Ni‘aj and Middle Bronze Age Tell el-Hayyat, located in the northern Jordan Valley, Jordan. These freshly augmented suites of carbonized seed dates now include 25 AMS dates from Tell Abu en-Ni‘aj and 31 AMS dates from Tell el-Hayyat. The modeled founding date for Tell Abu en-Ni‘aj strengthens an emerging high chronology for Early Bronze IV starting by 2500 cal BC, while the end of its habitation by 2200 cal BC may exemplify a regional pattern of increasingly pervasive abandonment among late Early Bronze IV settlements in the Southern Levant. In turn, our modeled date for the Early Bronze IV/Middle Bronze Age transition at Tell el-Hayyat around 1900 cal BC pushes this interface about a century later than surmised traditionally, and its abandonment in Middle Bronze III marks an unexpectedly early end date before 1600 cal BC. These inferences, which coordinate Bayesian AMS models and typological ceramic sequences for Tell Abu en-Ni‘aj and Tell el-Hayyat, contribute to an ongoing revision of Early and Middle Bronze Age Levantine chronologies and uncoupling of their attendant interpretive links between the Southern Levant and Egypt.

In paleoenvironmental research, several proxies are used to reconstruct climate and vegetation. The establishment of a chronological framework allows for the association of different proxies and correlation of events happening in different geographic areas. Cultural deposits, such as the shellmounds found along the coast of Brazil, play an important role in paleoenvironmental interpretations. Here, we have employed anthracological analysis in charcoal fragments from the Amourins shellmound, located at the margins of the Guanabara Bay, Rio de Janeiro. This allowed for the taxonomic identification and selection of short-lived trees and specific parts of plants for accurate radiocarbon dating. We recorded genera and families typical of the Atlantic Forest, restinga forest, open restinga and mangrove. The 14C ages of charred nuts from different occupational layers range from 3807 ± 35 to 3503 ± 70 BP and a sequential chronological model was built, relating the predominance of mangrove vegetation to the period between 4130–3960 cal BP.

Age disparities between charcoal samples and their context are a well-known problem in archaeological chronometry, and even small offsets could affect the accuracy of high-precision wiggle-matched dates. In many cases of taphonomic or anthropogenic loss of the outermost rings, sapwood-based methods for estimating cutting dates are not always applicable, especially with charcoal. In these instances, wiggle-matched terminus post quem (TPQ) dates are often reconciled with subjective or ad hoc approaches. This study examines the distribution of age disparities caused by ring loss and other factors in a large dendroarchaeological dataset. Probability density functions describing the random distribution of age disparities are then fit to the empirical distributions. These functions are tested on an actual wiggle-matched non-cutting date from the literature to evaluate accuracy in a single case. Simulations are then presented to demonstrate how an age offset function can be applied in OxCal outlier models to yield accurate dating in archaeological sequences with short intervals between dated episodes, even if all samples are non-cutting dates.

Calibrated radiocarbon (14C) determinations are commonly used in archaeology to assign calendar dates to a site’s chronological phases identified based on additional evidence such as stratigraphy. In the absence of such evidence, we can perform dense 14C sampling of the site to attempt to identify periods of heightened activity, separated by periods of inactivity, which correspond to archaeological phases and gaps between them. We propose a method to achieve this by hierarchical cluster analysis of the calibrated 14C dates, followed by testing of the different clustering solutions for consistency based on silhouette coefficient and statistical significance using randomization. Separate events identified in such a way can then be regarded as evidence for distinct phases of activity and used to construct a site-specific sequence. This can be in turn used as a Bayesian prior to further narrow down the distributions of the calibrated 14C dates. We assessed the validity of the method using simulated data as well as real-life archaeological data from the Bronze Age settlement of Troy. A Python implementation of the method is available online at https://github.com/demjanp/clustering_14C.

We here present a comparison of methods for the pretreatment of a batch of tree rings for high-precision measurement of radiocarbon at the Aarhus AMS Centre (AARAMS), Aarhus University, Denmark. The aim was to develop an efficient and high-throughput method able to pretreat ca. 50 samples at a time. We tested two methods for extracting α-cellulose from wood to find the most optimal for our use. One method used acetic acid, the other used HCl acid for the delignification. The testing was conducted on background 14C samples, in order to assess the effect of the different pretreatment methods on low-activity samples. Furthermore, the extracted wood and cellulose fractions were analyzed using Fourier transform infrared (FTIR) spectroscopy, which showed a successful extraction of α-cellulose from the samples. Cellulose samples were pretreated at AARAMS, and the graphitization and radiocarbon analysis of these samples were done at both AARAMS and the radiocarbon dating laboratory at Lund University to compare the graphitization and AMS machine performance. No significant offset was found between the two sets of measurements. Based on these tests, the pretreatment of tree rings for high-precision radiocarbon analysis at AARAMS will henceforth use HCI for the delignification.

The analysis of processing standards alongside samples for quality assurance in radiocarbon (14C) analyses is critical. Ideally, these standards should be similar both in nature and age to unknown samples. A new compound-specific approach was developed at the University of Bristol for dating pottery vessels using palmitic and stearic fatty acids extracted from within the clay matrix and isolated by preparative capillary gas chromatography. Obtaining suitable potsherds for use as processing standards in such analyses is not feasible, so we suggest that bog butter represents an ideal material for such purposes. We sampled ca. 450 g from two bog butter specimens and homogenized them by melting. We verified the homogeneity of both specimens by characterization of their lipid composition, δ13C values of individual lipids, and both bulk- and compound-specific radiocarbon analyses on 10 sub-samples of each bog butter specimen. The weighted means of all 14C measurements on the bog butter standards are 3777 ± 4 BP (IB33) and 338 ± 3 BP (IB38), thereby providing age-relevant standards for archaeological and historical fatty acids and ensuring the accuracy of radiocarbon determinations of lipids using a compound-specific approach. These new secondary standards will be subjected to an intercomparison exercise to provide robust consensus values.