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.

Obtaining accurate age determinations from minerals in archaeological ash is a major unsolved issue in radiocarbon (14C) dating. This is because the original 14C content of calcite, the main component of ash, is altered by isotopic exchange. Pyrogenic aragonite, another mineral phase recently discovered in ash, might preserve its 14C signature through time. Using a new method based on density separation and step combustion, we were able to isolate and date aragonitic ash from an archaeological destruction horizon of known age. Here we show that the 14C age of aragonite matches the age of the destruction horizon. Our results demonstrate that pyrogenic aragonite is a short-lived material suitable for 14C dating and directly related to human activities involving the use of fire, thus bearing major implications for the establishment of absolute chronologies for the past 50,000 yr.

The article reports the growth stop phenomenon, which was documented only for baobabs, i.e. for trees belonging to the Adansonia genus. The identification of growth stop was enabled by radiocarbon dating, which allows a complex investigation of samples collected from the trunk/stems of baobabs. In several cases, the outermost rings of baobabs, which were close to the bark, were found to be old, with ages of several hundreds of years, instead of being very young. Dating results of samples collected from six baobabs are presented. For multistemmed baobabs, the growth stop may occur only for one or several stems. We identified four factors that may induce the growth stop: (i) stress determined by severe climate conditions, (ii) old age, (iii) the need to keep a stable internal architecture, and (iv) the collapse of stems that survive this trauma. Baobabs and their stems affected by growth stop may survive for several centuries, by continuing to produce leaves, flowers, and fruits. This phenomenon was associated with the capacity of baobabs to store large amounts of water in their trunks/stems in the rainy season. This reservoir of water is used during the dry season and allows the trees to survive prolonged drought periods.

The Radiocarbon Laboratory of the Universidade Federal Fluminense, in Brazil, has been successfully applying the zinc reduction method for graphitization of carbon samples since the development of its early protocols in 2009. Successive methodological research aiming to improve and, ultimately, optimize the precision and accuracy of our results indicates that graphitization temperatures as low as 460°C promote erratic 13C isotopic fractionation, but an approximately constant fractionation of about –5‰ is achieved at 520°C. In this work, we present isotope ratio mass spectrometry (IRMS) δ13C results for 14C reference materials graphitized at 550°C with variable amounts of zinc. Based on the results obtained from the addition of 20, 35, and 50 mg of zinc, we conclude that a slightly lower variation in 13C isotope fractionation during graphitization is obtained with less zinc. Moreover, the average isotopic fractionation is not altered by increasing the graphitization temperature from 520°C to 550°C.

We identified human paleodietary changes from inhabitants of the Guanzhong basin since 8000 BP, based on published carbon and nitrogen isotopic measurements on bones, fauna and plant remains. We also directly measured 14C ages, δ13C and δ15N values from bones unearthed at the Zhouyuan site, west of Guanzhong, in order to reconstruct paleodietary changes of the ancient inhabitants. We found that during the Laoguantai period, animal foods were the main source of nourishment with supplementary plant-derived foods. After this period, plant-derived foods became the main food source, with supplementary animal sources. The development of dry farming led to increased consumption of foxtail millet and broomcorn millet. This trend persisted and marked a fundamental shift from hunting, gathering, and fishing to farming and animal domestication. The dietary trends of the ancient inhabitants also show pronounced regional differences through time. The use of domestic animals was proportionally higher in the eastern part of the Guanzhong region, while wild animals were more common in the west.

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.

Since the mid-19th century, rare prehistoric wooden carvings and human skeletal remains have been dredged from Pitch Lake, Trinidad, during commercial asphalt mining. Establishing a chronology for these objects is challenging, due to both a lack of stratigraphic and contextual information and the necessity to completely remove any pitch to ensure accurate radiocarbon (14C) dates. A range of solvent extraction protocols was tested to identify the most suitable one for pretreating the Pitch Lake artifacts, and then applied to ten wooden objects and a human cranium recovered from the lake. Several of these objects yielded earlier dates than expected, raising concerns that pitch had remained after pretreatment and had affected the dates. Pyrolysis-GC/MS and optical microscopy techniques were applied to material from the human cranium, a weaving tool, and a small bowl. These techniques, as well as routinely applied laboratory quality assurance procedures, indicated that there was no residual pitch within the cranium or the weaving tool after pretreatment, giving confidence to the dates. However, the small bowl was observed to still be contaminated with pitch after extensive pretreatment, indicating that the date is too old and can only be considered as a terminus post quem.

We report the chronological construction for the top portion of a speleothem, PC1, from southern Cambodia with the aim of reconstructing a continuous high-resolution climate record covering the fluorescence and decline of the medieval Khmer kingdom and its capital at Angkor (~9th–15th centuries AD). Earlier attempts to date PC1 by the standard U-Th method proved unsuccessful. We have therefore dated this speleothem using radiocarbon. Fifty carbonate samples along the growth axis of PC1 were collected for accelerator mass spectrometry (AMS) analysis. Chronological reconstruction for PC1 was achieved using two different approaches described by Hua et al. (2012a) and Lechleitner et al. (2016a). Excellent concordance between the two age-depth models indicates that the top ~47 mm of PC1 grew during the last millennium with a growth hiatus during ~1250–1650 AD, resulting from a large change in measured 14C values at 34.4–35.2 mm depth. The timing of the growth hiatus covers the period of decades-long droughts during the 14th–16th centuries AD indicated in regional climate records.

The Healy’s Lucky Strike site in central Alaska has an exceptional Holocene loess-paleosol sequence that has afforded us the ability to look at variation in 14C dating of soil organic matter (SOM) fractions in a high-latitude loess setting. Our work has focused on comparing the radiocarbon ages of charcoal and wood to base-soluble humic acids (HA) and base-insoluble soil residue (SR) fractions from bulk soil samples. Charcoal/wood ages were younger than HA ages reflecting the later stages of vegetation development at the surface of the soils prior to being covered by loess accumulation; the HA ages generally reflect the overall timing of soil formation and mean residence time of SOM. Soil residue ages are older than charcoal/wood and HA ages. SOM ages at this location become increasingly older than charcoal/wood ages with depth, reaching 750 to 8070 yr in difference and associated with weakly developed soils at the lowest depths. We suggest the drastic SOM age differences at this site result from the differential incorporation of small particles of coal throughout the sedimentary matrices introduced older contaminants to SR fractions.

Despite their great potential, charred particles of chaff-and-straw temper from daub architecture have very rarely been considered as material suitable for 14C dating. This short paper is intended to change this situation. With this aim in mind, we first present the rationale and objectives of the sampling procedure based on archaeobotanical exploration of prehistoric remains of daub architecture, and then report and discuss the results of a short chronometric exercise based on such samples. The empirical verification of the sampling procedure was based on finds related to the epi-Lengyel culture from Upper Silesia.

Studies using carbon isotopes to understand the global carbon cycle are critical to identify and quantify sources, sinks, and processes and how humans may impact them. 13C and 14C are routinely measured individually; however, there is a need to develop instrumentation that can perform concurrent online analyses that can generate rich data sets conveniently and efficiently. To satisfy these requirements, we coupled an elemental analyzer to a stable isotope mass spectrometer and an accelerator mass spectrometer system fitted with a gas ion source. We first tested the system with standard materials and then reanalyzed a sediment core from the Bay of Bengal that had been analyzed for 14C by conventional methods. The system was able to produce %C, 13C, and 14C data that were accurate and precise, and suitable for the purposes of our biogeochemistry group. The system was compact and convenient and is appropriate for use in a range of fields of research.

We report here on the radiocarbon performance on the AARAMS HVE 1MV Tandetron. 14C analysis is carried out in charge state 2+. We have avoided Li interference by appropriate settings of the high-energy electrostatic analyzer and the 30° second high-energy magnet. The 14C machine background is determined using unprocessed graphite, which yielded 58,650±2032 14C yr determined as the average and standard deviation of four measurements. International standards, which are used to monitor the long-term performance of the 14C measurements, agree with the reported consensus values.

The SUERC Radiocarbon Laboratory employs a one-step “background subtraction” method when calculating 14C ages. An interglacial wood (VIRI Sample K) is employed as the non-bone organic background standard, while a mammoth bone (LQH12) from Latton Quarry is used as the bone background standard. Results over several years demonstrate that the bone background is consistently around a factor of two higher and more variable than the wood background. As a result, the uncertainty on routine bone measurements is higher than for other sample types. This study investigates the factors that may contribute to the difference in F14C values and the higher variability. Preparations of collagen using modified Longin or ultrafiltration methods show no significant difference, nor does eliminating the collagen dissolution step. Two bone samples of known infinite age with respect to radiocarbon are compared and again no significant difference is observed. Finally, the quantity and age of the organic matter in the water used during the pretreatment is investigated and it is shown that there is insufficient organic matter in the reverse osmosis water to influence background values significantly. The attention is now on determining if incomplete demineralization could lead to contaminants being retained by the phosphate in the hydroxyapatite.

An accurate radiocarbon (14C) dating of mortars requires adjusting the sample preparation procedure to each specific mortar composition. In order to follow the influence of mortar components and the preparation procedure on dating results, a mortar intercomparison study (MODIS) was undertaken by 10 organizations (institutes and laboratories) in the analyses of four different types of mortars (see in this issue Hajdas et al. 2017 and Hayen et al. 2017). This paper presents the preparation protocol DoM v.1 applied by the Poznań team, together with dating results on a set of mortar samples used for the of intercomparison. This procedure involved petrographic observations, SEM-EDS analyses, different mechanical-chemical preparation, a test of leaching reaction for available fractions, and finally 14C dating of chosen samples. The applied preparation allows one to obtain dry-sieved grain fractions and different fractions from suspension: grain fractions from suspension collected in different times of leaching, repeated suspension (different portions), as well as suspension collected at different times of sedimentation. The obtained results show the great importance of good sampling and the influence of sample preparation on 14C dating results.

Radiocarbon ages were determined on different fractions extracted from buried paleosols in south-central Alaska as an experiment to establish best practices for analysis of low-organic-matter paleosols. Seven samples were collected from directly beneath tephra deposits to determine the eruption frequency of Mount Spurr Volcano, Alaska. Soil development near the volcano is poor due to the high-latitude climate and frequent burial of soil surfaces by tephra. Contamination of soils by local wind-blown material is a concern. The humic acid 14C ages are consistently younger than both the bulk soil and residue after extraction ages. The difference in ages between the humic acid extract and bulk soil range from 60–1130 14C yr BP and 180–4110 14C yr BP, respectively, for residue. Previous observations from dating different soil fractions show that residue ages are typically younger than humic acid extracts presumably because they contain a fraction of younger plant material including roots. We attribute the older ages to contamination by old carbon from eolian charcoal particles. This study supports the use of accelerator mass spectrometry (AMS) 14C dating of the humic acid fraction in order to estimate the age of soil that presumably marks the age of burial and avoids suspected contamination by old carbon.

Accelerator systems designed for a wide variety of ion beam analysis (IBA) applications usually have a multitude of beamline components and long beam lines. In the use of these systems, beam optimization is especially important for attaining high-precision accelerator mass spectrometry (AMS) results. The optimization involves multiple parameters, dependencies between parameters, and multiple optimization targets. To improve the repeatability and reliability of AMS results, we have developed a profiling program for automatic beam optimization. In our implementation, the accelerator control parameters, measured beam currents, and AMS detector count rates are all stored in a real-time database. The profiling routine can scan any accelerator parameter and fetch from the database the profile of any measured quantity as a function of the parameter. The routine is usually used to scan over roughly 20 essential parameters of the system and setting them to the optimum values. Automatic optimization is fast, easy to use, robust to noise, and gives reproducible results. In addition, the graphical output in the form of current and count rate profiles is highly informative. Automatic optimization together with other improvements to the AMS setup have enabled us to push the precision of the system to better than 0.2%.

The Cave of Pan is located on the N/NE slope of the hill of Oinoe (38°09′31.60′′N, 23°55′48.60′′E), west of modern Marathon. In rescue excavation campaigns during the last three years, among other finds, charcoal and seashell samples were also collected. The purpose of this study is the accelerator mass spectrometry (AMS) dating of the cave’s anthropogenic deposits and the calculation of the regional marine reservoir effect during the Neolithic period. For that purpose, 7 charcoal pieces and 1 seashell were dated. Our results show that the cave was used from the second quarter of the 6th millennium (Middle Neolithic period) until the beginning of the 5th millennium BC. Additionally, one sample collected from a depth of 2 cm from the present surface of the cave yielded an age falling within the 6th century AD, giving thus the absolute time span of the cave use. Moreover, the radiocarbon (14C) ages of one pair of charcoal-seashell samples showed that the marine reservoir age R(t) in the estuarine Marathon Bay region during the 5th millennium BC is 775±57 yr and the local sea surface reservoir deviation ΔR is found to be 402±63 14C yr (within 1σ).

Nitrogenous compounds of soil organic matter constitute a major N reservoir on Earth. Both the world food protein supply produced by agriculture and the global contamination by reactive nitrogen species rely on the dynamics of these compounds. To investigate their dynamics, we used both natural 13C labeling and accelerator mass spectrometry (AMS) 14C dating of the α-carboxyl amino carbon, which is specific of the amino acid fraction that was extracted from bulk soil organic matter by ninhydrin hydrolysis. We applied this isotopic approach to investigate the age of carboxyl carbon in a maize-cultivated Cambisol chronosequence. Based on a few measurements, we demonstrate the feasibility of this new compound-specific method of investigation of soil carbon dynamics. We show that soil organic matter amino acids can be split into two very distinct dynamic compartments: the majority having a mean age of a few years and a minority having a mean carbon age of several millennia. The latter fraction can be either strongly stabilized in soils, or can arise from microbial utilization of old carbon resources, as predicted by the priming effect theory.