Radiocarbon (14C) dating of sediment deposition around Antarctica is often challenging due to heterogeneity in sources and ages of organic carbon in the sediment. Chemical and thermochemical techniques have been used to separate organic carbon when microfossils are not present. These techniques generally improve on bulk sediment dates, but they necessitate assumptions about the age spectra of specific molecules or compound classes and about the chemical heterogeneity of thermochemical separations. To address this, the Rafter Radiocarbon Laboratory has established parallel ramped pyrolysis oxidation (RPO) and ramped pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) systems to thermochemically separate distinct carbon fractions, diagnose the chemical composition of each fraction, and target suitable RPO fractions for radiocarbon dating. Three case studies of sediment taken from locations around Antarctica are presented to demonstrate the implementation of combined RPO-AMS and Py-GC-MS to provide more robust age determination in detrital sediment stratigraphy. These three depositional environments are good examples of analytical and interpretive challenges related to oceanographic conditions, carbon sources, and other factors. Using parallel RPO-AMS and Py-GC-MS analyses, we reduce the number of radiocarbon measurements required, minimize run times, provide context for unexpected 14C ages, and better support interpretations of radiocarbon measurements in the context of environmental reconstruction.

This work presents the integration of an elemental analyzer (EA) and an isotope ratio mass spectrometer (IRMS) into the 6 MV AMS system at the Institute for Nuclear Physics, University of Cologne. The AMS measurement of δ13C values for IAEA-C6 reference material resulted in –11.39(226)‰, compared to –10.28(32)‰ obtained by IRMS. The EA-IRMS system was also tested with IAEA-C3, IAEA-C5, and IAEA-C7 reference materials, yielding –24.79(9), –25.18(15), and –14.76(18)‰ respectively. Compared to the IAEA information values given as –24.91(49), –25.49(72) and –14.48(21)‰ respectively. To investigate an observed sample mass dependency, environmental samples from Spitzbergen were examined, showing δ13C values of –25.17(55), –25.80(31), and –26.17‰ in Cologne, while Hamburg recorded –24.8(1), –25.5(1), and –26.2(13)‰. In summary, this new setup could enable online analysis and quasi-simultaneous measurements of 14C, δ13C, and δ15N for ultra-small samples, utilizing precise δ13C values from IRMS for fractionation correction of the 14C/14C isotopic ratio.

The fifth season of excavations of Oponice Castle in 2020 was located in the lower castle’s courtyard. The research led to discovery of an original clay floor being heavily burned with charred plank and a rectangular stone-brick construction. The construction has collapsed upper part with a fallen low brick arch. The whole area was covered with numerous stove tiles and one clay mold for the production of stove tiles. The construction was identified as a pottery kiln dated to the second half of the 16th until the first half of the 17th century AD by the findings from excavated layer identified to the kiln destruction. Also, written sources mention a large fire in 1645 which destroyed the castle. The aim of this article is to use different methods of dating and refine the chronology of the context through microarchaeology and Bayesian modeling. For these purposes different types of samples were collected. The sampling focused on site formation process determination of pottery kiln use and the way of its destruction. Applying Bayesian analysis improved overall dating, through modeled time interval of the three individual sequences and helped recreated historical events during the period, when the calibration curve fluctuates.

Accurate radiocarbon (14C) analysis depends on a successful carbon separation relevant to the studied object. The process of 14C dating involves the following steps: characterization and sample choice, sample treatment, measurements, and evaluation of the results. Here, we provide an overview of conventional approaches to macromolecular samples and address specific issues such as detecting and removing contamination with roots, dolomite, and conservation products. We discuss the application of elemental analysis (%N, %C) in the preparation of bones and the infrared analysis in monitoring the contamination of samples. Our observations provide the basis for the discussions of the existing results and for planning the future sampling.

An archaeological excavation conducted on U Kasáren St. in the Prague Castle area (Czech Republic) in 2020 revealed the remains of a medieval settlement consisting of houses of different constructions (pit dwelling, masonry construction), pyrotechnical (possibly metallurgical) features and unspecified pits. The excavation also revealed evidence of fire events and traces of viniculture on the outskirts of the Prague Castle area. Archaeological data allowed only a rough dating of the investigated settlement in the 10th–13th centuries. This paper presents the results of the radiocarbon dating of various materials (animal bones, archaeobotanical samples) from the settlement features and the contribution of the results to the clarification of the chronology of the site.

The Laboratoire des Sciences du Climat et de l’Environnement (LSCE) has operated a radiocarbon dating laboratory for almost 70 years. It has evolved from a traditional ß-decay counting to an accelerator mass spectrometry facility. In 2015, the LSCE received a major upgrade with the installation of a MICADAS. This evolution required adjustments in sample preparation to match the new capability to date samples as small as a few tens of µgC. We summarize here the sample cleaning procedures and the chemical purification or extraction treatment that we apply to the samples. We also report values of blank and reference materials of different matrices that match the large diversity of samples handled at LSCE.

After an intercomparison age experiment carried out in the framework of the first MODIS (MOrtar Dating Inter-comparison Study) project, the results showed general agreement both between optically stimulated luminescence (OSL) dating laboratories and with radiocarbon (14C) dating results. As the needs for the selection of samples convenient for an inter-comparison are not the same between 14C and OSL, for the second running, it has been decided to choose two different sample sets, one to share between the radiocarbon labs and one for the OSL dating ones. The results obtained by applying different experimental protocols (multigrain and single grain techniques) and different statistical models (weighted mean, central age mode, average dose model, minimum age model and exponential exposure dose) are discussed in this work.

Quicklime samples were collected from six vertical layers (L1–L6) of a feedstock calcined in a traditional single-batch wood-fired kiln and assessed. Three samples were well-burned and three under-burned. The quicklime was slaked in an excess of water and the presence of unburned particles was investigated after settling it into putty. The putty was assessed as bulk and also at three depth levels. Thermal analysis determined the CO2 residua in the quicklime samples. Cathodoluminescence detected individual unburned particles and image analysis was used for their quantification. Settling of the putties led to a considerable reduction of geogenic particles in the layers above the bottom. This was also confirmed by the stable isotope analysis. In the case of the putties made from well-burned quicklime, the δ13C values of samples L4 and L5 ranged from –25.5‰ to –20.5‰ VPDB, and the δ18O values ranged from –17.5‰ to –16.5‰ VPDB. The fractionation was likely affected by the division according to the particle size during the sedimentation. The results of the 14C analysis correlate with the quantified percentage of cathodoluminescent particles.

This paper compares various wood pretreatment methods for highly degraded, and problematic fossil wood extracted from the opencast Szczerców site of the Bełchatów Lignite Mine in Central Poland. The study evaluates the pretreatment methods using both large samples (55–255 g, referred to as series A) and small samples (36–150 mg, referred to as series B). Additionally, all preparation methods were applied to medium-sized samples (approximately 3 g, referred to as series C) with solvent washes in the Soxhlet apparatus. Radiocarbon dating was conducted using the LSC technique (subseries A1) and the AMS technique (subseries A2, series B, and C). The effectiveness and utility of each pretreatment protocol were compared based on 14C measurements and FTIR analysis. Through the conducted research and a multi-criteria analysis, the most effective method for preparing old fossil wood was identified. Our experience indicates that an extended, multistage preparation of highly degraded fossil wood samples, with a 14C concentration near the detection limit of the radiocarbon method, may result in a significant increase in 14C content.

Obtaining accurate radiocarbon (14C) results from wood samples requires the extraction of cellulose. In the past, this has been done using different combinations of methods including acidified bleaching, acid-base-acid, and strong bases. This often becomes a time-consuming task in most analyses, especially when single ring isotope chronologies are needed from wood samples. Using 14C and Fourier-transform infrared spectroscopy (FTIR), we tested four different pretreatment methods to determine their ability to produce high quality cellulose. We then adjusted the best methods to determine a method for pretreating wood laths of multiple rings. A sequence of base-acid-base-acid-bleach + strong base (BABAB+) and BABAB produced the most accurate results when compared to the Bomb20 Northern Hemisphere Zone 1 curve with an average difference in Δ14C of 1.3‰ and 5.8‰ respectively. These methods were adjusted to pretreat an entire wood lath and a comparison of the FTIR results suggest that our adjusted BABAB+ and BABAB produced high quality cellulose comparable to that of an individually pretreated ring. The possibility to pretreat wood lath samples has the potential to more than double the number of tree rings which can be pretreated in a week. This is a significant reduction in time when creating long tree ring chronologies.

Since the first developments of anthropogenic lime materials radiocarbon (14C) dating in the 1960s, numerous studies have been undertaken and developed to investigate the topic further. Historic mortars are complex composite and open system materials that can incorporate a large range of components. Due to the complexity of the historic lime mortars composition, they are not part of a routine protocol in most radiocarbon laboratories and reliable dating is not always achieved. A thorough characterization needs to be performed and different preparation methods can be considered as a function of their compositions. A vast range of terms are employed to qualify the lime mortars components and alterations that can possibly have an influence on the dating result. Here, a detailed description of these components and the various terms used is listed. To illustrate this, images obtained by thin-section petrography and cathodoluminescence are presented in addition to radiocarbon results using stepwise acid hydrolysis on Belgian mortars having different provenance, state, age and composition. Depending on the type of aggregate used, the type of binder and its conservation state, the eventual presence of weathering carbonates and the assumed speed of the carbonation process, the reliability of radiocarbon measurements using the stepwise acid hydrolysis technique is discussed and confronted with presumed historical constraints.

Shipping radiocarbon samples from the scientist to the laboratories involves packaging and wrapping them with all sorts of bags and materials to make sure the samples arrive safely. Over the years a variety of possible and impossible package materials have arrived at our laboratory, causing problems occasionally but often being the highlight of the day cheering up the people involved. The reality of excavating important, occasionally unexpected, samples during field work sometimes includes taking samples when time is short or package materials could not be prepared. At this point, any kind of package becomes useful. Things like cigarette packets, reused office packets, tissue boxes, or medical packaging can become handy. But sometimes samples are taken, wrapped in aluminum foil, and forgotten in the desks. This article celebrates creativity, giving an overview of the many ways samples can be packed. However, using some of the less-than-ideal choices, drawbacks will be shown and possible problems explained.

The radiocarbon (14C) dating method was applied to a survey of treasured items related to the ruins of the Imperial Residence in Anou, Nara Prefecture, which was one of the capitals of Japan during the 14th century. In this work, we dated two storage bags for Japanese musical instruments that are believed to be from the period of Emperor Go-Daigo who established the Southern Court. The 14C dating of these treasures proved that the musical instrument sacks are contemporaneous with the dating of the Imperial Residence ruins designated as an Important Cultural Property of Japan. In addition, there are limited surviving examples of silk fabrics from the Middle Ages compared to the Ancient and Early Modern periods, making this a valuable resource in the history of silk fabrics in Japan.

Although paleomagnetic secular variations (PSV) often corroborate radiocarbon (14C)-based lacustrine sediment chronologies, this is not the case at the high-altitude site Khar Nuur in the Mongolian Altai Mountains. Our results show that the inclination pattern resembles those from a regional reference record from Shireet Naiman Nuur and global geomagnetic field models very well, but with a constant offset of 730 ± 90 yr. Possible reservoir effects from terrestrial pre-aging and hardwater effects can be excluded as the cause of the ∼730-yr offset because the different dated compounds correspond very well to each other, and modern reservoir effects are negligible. Instead, the constant ∼730-yr offset in the PSV pattern is likely the result of a constant lock-in depth of 26 ± 2 cm below the sediment-water interface at Khar Nuur. This assumption is supported by comparison of paleoclimatological proxies from Shireet Naiman Nuur, where similarities are obvious for the 14C-based chronology of Khar Nuur without a ∼730-yr adjustment. Therefore, the previously published 14C-based chronology of Khar Nuur provides a reliable age control. Accepting the lock-in depth of 26 ± 2 cm, the good consistency in inclination between Khar Nuur and global geomagnetic field models highlights the reliability of the latter even in a paleomagnetically understudied area.

Accelerator mass spectrometry (AMS) radiocarbon (14C) dating is central to the development of robust chronologies in archaeological and paleoenvironmental contexts spanning the last 50,000 years. For dates to be accurate, samples must be free of exogenous carbon contamination. At the Oxford Radiocarbon Accelerator Unit (ORAU), considerable advancements in the dating of bone collagen have been made through the development of a high performance liquid chromatography (HPLC) method for the dating of the amino acid hydroxyproline, which can mitigate the effects of carbon contamination. However, recent changes in ligand manufacturing methods for the mixed-mode column used in the ORAU protocol (Primesep A, SIELC Technologies; IL, USA) have resulted in unacceptably high analytical backgrounds. Prior to the manufacturing change, backgrounds of > 50k BP were achievable. Since the manufacturing change, a mean background of 32.5k BP has been measured. Due to column bleed, the Primesep A is therefore no longer suitable for 14C measurement of hydroxyproline from older material. Here, we present background data and the chromatography conditions used to isolate hydroxyproline using an alternative column, a preparative-scale Newcrom AH, which shows promising potential as an alternative for the routine isolation and AMS dating of hydroxyproline—especially approaching the age and mass limits of the method.

The IntCal family of radiocarbon (14C) calibration curves is based on research spanning more than three decades. The IntCal group have collated the 14C and calendar age data (mostly derived from primary publications with other types of data and meta-data) and, since 2010, made them available for other sorts of analysis through an open-access database. This has ensured transparency in terms of the data used in the construction of the ratified calibration curves. As the IntCal database expands, work is underway to facilitate best practice for new data submissions, make more of the associated metadata available in a structured form, and help those wishing to process the data with programming languages such as R, Python, and MATLAB. The data and metadata are complex because of the range of different types of archives. A restructured interface, based on the “IntChron” open-access data model, includes tools which allow the data to be plotted and compared without the need for export. The intention is to include complementary information which can be used alongside the main 14C series to provide new insights into the global carbon cycle, as well as facilitating access to the data for other research applications. Overall, this work aims to streamline the generation of new calibration curves.

CH4 is the second most important anthropogenic greenhouse gas and originates from different sources. The use of radiocarbon (14C) analysis of CH4 opens up the possibility to differentiate geological and agricultural origin. At the CologneAMS facility, the demand for 14C analysis of CH4 required the development of a sample handling routine and a vacuum system that converts CH4 to CO2 for direct injection of CO2 into the AMS. We evaluated the processing of CH4 using several series of gas mixtures of 14C-free and modern standards as well as biogas with sample sizes ranging from 10 to 50 µg C. The results revealed a CH4 to CO2 conversion efficiency of 94–97% and blank values comparable to blank values achieved with our routinely used vacuum system for processing CO2 samples. The tests with a near modern CH4:CO2 biogas mixture gave reproducible results with a near modern 14C content of 0.967–1.000 F14C, after applying the background correction.

We constructed a laser ablation (LA) system using a diode laser for the accelerator mass spectrometry radiocarbon (AMS 14C) measurement of organic materials. The system could extract adequate CO2 to analyze small masses (0.1 mg C) at a resolution of 250 µm by a 5.5 W diode laser. The LA system was assessed using standard materials (IAEA-C1, IAEA-C2, IAEA-C3, IAEA-C6, and Ox II) and applied to natural tree ring samples. For the LA sampling of organic samples, which generally results in incomplete combustion, tungsten (VI) oxide was used as an oxidant to achieve complete burning. The results of the measurement of standard materials showed a low 14C background of F14C 0.0085 ± 0.0005 and reasonable reproduction of 14C values. Finally, we applied this system to a single-year analysis of tree-ringed spruce timber in Alaska. It was observed to have a detectable background for the 14C bomb peak.

Radiocarbon (F14C) and stable carbon (δ13C) values were measured in single grains of spring barley (Hordeum vulgare L.) from the sample archive from two adjacent sites of the Long-term Experiments (LTEs) Hoosfield Spring Barley at Rothamsted Research (Harpenden, Hertfordshire, UK), covering the growing periods (March to September) of 1852 to 2020. F14C data of the barley grain confirm that recent values are approaching and will decline below the “nominal” F14C value of 1, tracking a similar decrease reported in other studies. Importantly, the measured δ13C values reveal a different temporal decline over the pre-bomb and post-bomb timescale. Detailed statistical analysis of δ13C data along with δ13C analysis of independent, archived barley mash samples, verifies and quantifies the extent and rate of this decline. Evidence presented from the barley grain and barley mash samples suggests a clear breakpoint in δ13C data occurring in 1995, where the rate of change alters, in that the slope in δ13C data for the pre-1995 period is declining at 1.4‰ per century, and the slope in δ13C for the post-1995 period is declining at 3.6‰ per century. Such a consistent shift in δ13C data could be used with F14C values to extend the use of the bomb peak for forensic, ecological, and environmental applications.

In this study, we investigate the distribution of radiocarbon and uranium in the calcified opercula of Turbo sp. collected from Ryukyu region and Chiba, Japan, to explore the potential of U/Th dating using mollusks collected from the Japanese archipelago. We acquired high-resolution radiocarbon and uranium concentration measurements using single-stage accelerator mass spectrometry and laser ablation−inductively coupled plasma−mass spectrometry. Our results show that uranium in the opercula of modern Turbo sp. is unevenly distributed at concentrations 1000 times less than those in coral skeletons. Radiocarbon found in the calcified opercula samples record ambient seawater radiocarbon values as well as coral skeletons. Uranium in the calcified opercula of Holocene Turbo marmoratus were also unevenly distributed and concentrated within the opercula in a different manner than observed in modern samples, suggesting uranium exchange after death. Our results suggest variable uptake of uranium isotopes into mollusk shells and highlights the need for rigorous sample selection criteria when choosing mollusks species for U/Th dating around Japan.