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A newly developed compact AMS, LEA (Low Energy Accelerator), is tested and compared with a state-of-the-art AMS system MICADAS (Mini Carbon Dating System), which has a precision performance of better than 1‰ for modern 14C. The main difference between these two systems is the acceleration voltage, which has been reduced from 200 kV with the MICADAS system to 50 kV with the LEA system. In order to execute the final performance tests, exactly same samples (2 sets consisting of 7 standards, 4 blanks, 26 wood samples) are measured on both systems successively. The results show that the LEA system is fully operational, and the performance is entirely comparable with that of the MICADAS system.
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.
Nowadays, most radiocarbon (14C) laboratories can reliably avoid and remove any possible sample contamination during the pretreatment of organic samples (e.g., bones, charcoal, or trees) thanks to a series of methods commonly used by the radiocarbon community. However, what about the final step, the storage of graphite? Rarely do the laboratories produce their graphite and ship it as pressed targets to accelerator mass spectrometry (AMS) facilities for measurement. Pressed graphite in aluminum targets are vulnerable to contamination, and during shipment or storage, exogenous carbon can be introduced again. Here we report a test on various archaeological sample materials from different environments and different periods (from the past three millennia to the Middle Paleolithic period). We transformed them into graphite, pressed the graphite into targets and sent them to two different AMS laboratories to be dated. We observe that packing details of the targets, extended shipment and storage time may lead to contamination which can be avoided by appropriate packaging in tight metal cans and sealed in vacuum bags. Close cooperation and coordination between our chemistry laboratory and the AMS facilities, high standards in contamination removal, and efficient measurement planning enabled us to obtain reliable 14C ages within a short time.
A high-resolution multiproxy lake sediment dataset, comprising lithology, radiography, μXRF elemental, magnetic susceptibility (MS), δ13C, and δ18O measurements since ca. AD 400 is presented in this study. Changes in lithology, radiography, magnetic susceptibility (MS), δ13C, and δ18O reflect wet/dry climate periods, whereas variability in log(Ca/K) can reflect warm/cold climate periods. Analyses of the multiproxy results allow the distinction of several climate periods, which may be associated with climatic phenomena such as changes in North Atlantic Oscillation (NAO) and/or solar activity. The influence of NAO−/NAO+ (negative/positive) is suggested to be related with the southward/northward displacement of the storm tracks resulting from the NAO−/NAO+ phases. For solar activity, the influence is explained through a direct increase in solar heating leading to calcite precipitation. The Dark Ages Cold Period (DACP, AD 450–750) reflects cold-dry climate conditions at this site, indicative of a positive North Atlantic Oscillation (NAO+) and low solar activity. The Medieval Climate Anomaly (MCA, AD 950–1250) exhibits wet-dry-wet and warm-cold-warm climate conditions. The wet/dry periods likely are associated with NAO−/NAO+, respectively, and the warm/cold period may reflect relatively high/low solar activity. The Little Ice Age (LIA, AD 1400–1850) is characterized by dry and cold climate conditions, suggesting the influence of NAO+ and low solar activity. Comparison of the results of this study with local and regional results suggests a generally similar climate pattern, which is indicative of similar climate mechanisms. The contradictions can be associated with age-related uncertainties, orographic differences, and/or other regional teleconnections.
Radiocarbon observations (Δ14C) in dissolved inorganic carbon (DIC) of seawater provide useful information about ocean carbon cycling and ocean circulation. To deliver high-quality observations, the Laboratory of Ion Beam Physics (LIP) at ETH-Zurich developed a new simplified method allowing the rapid analysis of radiocarbon in DIC of small seawater samples, which is continually assessed by following internal quality controls. However, a comparison with externally produced 14C measurements to better establish an equivalency between methods was still missing. Here, we make the first intercomparison with the National Ocean Sciences Accelerator Mass Spectrometry (NOSAMS) facility based on 14 duplicate seawater samples collected in 2020. We also compare with prior deep-water observations from the 1970s to 1990s. The results show a very good agreement in both comparisons. The mean Δ14C of 12 duplicate samples measured by LIP and NOSAMS were statistically identical within one sigma uncertainty while two other duplicate samples agreed within two sigma. Based on this small number of duplicate samples, LIP values appear to be slightly lower than the NOSAMS values, but more measurements will be needed for confirmation. We also comment on storage and preservation techniques used in this study, including the freezing of samples collected in foil bags.
Plasma oxidation for 14C sampling utilizes low-pressure (133 Pa), low-energy (<50 W), and low- temperature (<50°C) Ar- and O2-plasmas generating CO2 for AMS dating. O2-plasmas on empty chambers remove organic contamination. When clean, a new specimen is inserted and Ar-plasmas dislodge adsorbed atmospheric CO2 from surfaces. Finally, O2-plasmas oxidize organic materials to CO2 for AMS analysis. During some Ar-plasmas we observed anomalous pressure increases and unexpectedly high CO2. Residual gas analysis detected water, hydrogen and oxygen species with Ar and CO2 indicating water plasmas that produced excited oxygen species that prematurely oxidized specimen organic matter. Evolution of excess CO2 during Ar cleaning compromises the ability to affirm that atmospheric CO2 was removed. Standards, TIRI Belfast Pine and VIRI I Whalebone, were dated to determine whether water-induced oxidation was a confounding influence in dating. TIRI wood was sampled twice, once a water-soaked specimen in an Ar plasma and once with water-vapor-plasma only. The TIRI dates agreed with six earlier dates on usual specimens. A colloidal extract from VIRI I whale bone was also sampled and dated twice using both water–plasma oxidation in an Ar-plasma and in an O2-plasma. Dating agreement suggests that water plasmas do not pose undue risks of contamination.
The Chronos 14Carbon-Cycle Facility is a new radiocarbon laboratory at the University of New South Wales, Australia. Built around an Ionplus 200 kV MIni-CArbon DAting System (MICADAS) Accelerator Mass Spectrometer (AMS) installed in October 2019, the facility was established to address major challenges in the Earth, Environmental and Archaeological sciences. Here we report an overview of the Chronos facility, the pretreatment methods currently employed (bones, carbonates, peat, pollen, charcoal, and wood) and results of radiocarbon and stable isotope measurements undertaken on a wide range of sample types. Measurements on international standards, known-age and blank samples demonstrate the facility is capable of measuring 14C samples from the Anthropocene back to nearly 50,000 years ago. Future work will focus on improving our understanding of the Earth system and managing resources in a future warmer world.
Northern and southern hemispheric influences—particularly changes in Southern Hemisphere westerly winds (SSW) and Southern Ocean ventilation—triggered the stepwise atmospheric CO2 increase that accompanied the last deglaciation. One approach for gaining potential insights into past changes in SWW/CO2 upwelling is to reconstruct the positions of the northern oceanic fronts associated with the Antarctic Circumpolar Current. Using two deep-sea cores located ~600 km apart off the southern coast of Australia, we detail oceanic changes from ~23 to 6 ka using foraminifer faunal and biomarker alkenone records. Our results indicate a tight coupling between hydrographic and related frontal displacements offshore South Australia (and by analogy, possibly the entire Southern Ocean) and Northern Hemisphere (NH) climate that may help confirm previous hypotheses that the westerlies play a critical role in modulating CO2 uptake and release from the Southern Ocean on millennial and potentially even centennial timescales. The intensity and extent of the northward displacements of the Subtropical Front following well-known NH cold events seem to decrease with progressing NH ice sheet deglaciation and parallel a weakening NH temperature response and amplitude of Intertropical Convergence Zone shifts. In addition, an exceptional poleward shift of Southern Hemisphere fronts occurs during the NH Heinrich Stadial 1. This event was likely facilitated by the NH ice maximum and acted as a coup-de-grâce for glacial ocean stratification and its high CO2 capacitance. Thus, through its influence on the global atmosphere and on ocean mixing, “excessive” NH glaciation could have triggered its own demise by facilitating the destratification of the glacial ocean CO2 state.
A coupled accelerator mass spectrometer–gas interface system has been successfully operating at the Hertelendi Laboratory of Environmental Studies, Debrecen, Hungary, since 2013. Over the last 6 years more than 500 gas targets were measured below 100 µg carbon content for carbon isotopic composition. The system was tested with blanks, OxII, IAEA-C1, IAEA-C2, and IAEA-C7 standards. The performance of our instrumentation shows good agreement with other published gas-interface system data and also shows a quite good agreement with the nominal value of international standard samples. There is a measurable but quite small memory effect after modern samples, but this does not significantly affect the final results. Typical ion currents at the low energy side were between 10–15 µA with a 5% CO2 in He mixing ratio. The relative errors average ±6% for samples greater than or equal to 10 µgC sample with mean count rates of 300 counts per microgram C for OxII. The blank is comparable with other systems, which is 0.0050 ± 0.0018 F14C or 34,000–47,000 yr BP, which allows for the routine measurement of both of small environmental and archeological samples.
Radiocarbon (14C) ages cannot provide absolutely dated chronologies for archaeological or paleoenvironmental studies directly but must be converted to calendar age equivalents using a calibration curve compensating for fluctuations in atmospheric 14C concentration. Although calibration curves are constructed from independently dated archives, they invariably require revision as new data become available and our understanding of the Earth system improves. In this volume the international 14C calibration curves for both the Northern and Southern Hemispheres, as well as for the ocean surface layer, have been updated to include a wealth of new data and extended to 55,000 cal BP. Based on tree rings, IntCal20 now extends as a fully atmospheric record to ca. 13,900 cal BP. For the older part of the timescale, IntCal20 comprises statistically integrated evidence from floating tree-ring chronologies, lacustrine and marine sediments, speleothems, and corals. We utilized improved evaluation of the timescales and location variable 14C offsets from the atmosphere (reservoir age, dead carbon fraction) for each dataset. New statistical methods have refined the structure of the calibration curves while maintaining a robust treatment of uncertainties in the 14C ages, the calendar ages and other corrections. The inclusion of modeled marine reservoir ages derived from a three-dimensional ocean circulation model has allowed us to apply more appropriate reservoir corrections to the marine 14C data rather than the previous use of constant regional offsets from the atmosphere. Here we provide an overview of the new and revised datasets and the associated methods used for the construction of the IntCal20 curve and explore potential regional offsets for tree-ring data. We discuss the main differences with respect to the previous calibration curve, IntCal13, and some of the implications for archaeology and geosciences ranging from the recent past to the time of the extinction of the Neanderthals.
We undertook a strengths, weaknesses, opportunities, and threats (SWOT) analysis of Northern Hemisphere tree-ring datasets included in IntCal20 in order to evaluate their strategic fit with the demands of archaeological users. Case studies on wiggle-matching single tree rings from timbers in historic buildings and Bayesian modeling of series of results on archaeological samples from Neolithic long barrows in central-southern England exemplify the archaeological implications that arise when using IntCal20. The SWOT analysis provides an opportunity to think strategically about future radiocarbon (14C) calibration so as to maximize the utility of 14C dating in archaeology and safeguard its reputation in the discipline.
Early researchers of radiocarbon levels in Southern Hemisphere tree rings identified a variable North-South hemispheric offset, necessitating construction of a separate radiocarbon calibration curve for the South. We present here SHCal20, a revised calibration curve from 0–55,000 cal BP, based upon SHCal13 and fortified by the addition of 14 new tree-ring data sets in the 2140–0, 3520–3453, 3608–3590 and 13,140–11,375 cal BP time intervals. We detail the statistical approaches used for curve construction and present recommendations for the use of the Northern Hemisphere curve (IntCal20), the Southern Hemisphere curve (SHCal20) and suggest where application of an equal mixture of the curves might be more appropriate. Using our Bayesian spline with errors-in-variables methodology, and based upon a comparison of Southern Hemisphere tree-ring data compared with contemporaneous Northern Hemisphere data, we estimate the mean Southern Hemisphere offset to be 36 ± 27 14C yrs older.
Annually resolved tree-ring samples of the time period 1625–1510 BCE were analyzed from the German oak tree-ring chronology. Blocks of the same tree rings were previously used to generate IntCal calibration data. The new dataset shows an offset to the calibration data IntCal13 of 24 years and resembles annual data for the same time period derived from tree-ring records in other growth locations. A subset of samples of the period 1625–1585 BCE was additionally measured in three other laboratories (ETH, AAR, AA) for quality control.
As the worldwide standard for radiocarbon (14C) dating over the past ca. 50,000 years, the International Calibration Curve (IntCal) is continuously improving towards higher resolution and replication. Tree-ring-based 14C measurements provide absolute dating throughout most of the Holocene, although high-precision data are limited for the Younger Dryas interval and farther back in time. Here, we describe the dendrochronological characteristics of 1448 new 14C dates, between ~11,950 and 13,160 cal BP, from 13 pines that were growing in Switzerland. Significantly enhancing the ongoing IntCal update (IntCal20), this Late Glacial (LG) compilation contains more annually precise 14C dates than any other contribution during any other period of time. Thus, our results now provide unique geochronological dating into the Younger Dryas, a pivotal period of climate and environmental change at the transition from LG into Early Holocene conditions.
In 2018 Pearson et al. published a new sequence of annual radiocarbon (14C) data derived from oak (Quercus sp.) trees from Northern Ireland and bristlecone pine (Pinus longaeva) from North America across the period 1700–1500 BC. The study indicated that the more highly resolved shape of an annually based calibration dataset could improve the accuracy of 14C calibration during this period. This finding had implications for the controversial dating of the eruption of Thera in the Eastern Mediterranean. To test for interlaboratory variation and improve the robustness of the annual dataset for calibration purposes, we have generated a replicate sequence from the same Irish oaks at ETH Zürich. These data are compatible with the Irish oak 14C dataset previously produced at the University of Arizona and are used (along with additional data) to examine inter-tree and interlaboratory variation in multiyear annual 14C time-series. The results raise questions about regional 14C offsets at different scales and demonstrate the potential of annually resolved 14C for refining subdecadal and larger scale features for calibration, solar reconstruction, and multiproxy synchronization.
As part of the ongoing effort to improve the Northern Hemisphere radiocarbon (14C) calibration curve, this study investigates the period of 856 BC to 626 BC (2805–2575 yr BP) with a total of 403 single-year 14C measurements. In this age range, IntCal13 was constructed largely from German and Irish oak as well as Californian bristlecone pine 14C dates, with most samples measured with a 10-yr resolution. The new data presented here is the first atmospheric 14C single-year record of the older end of the Hallstatt plateau based on an absolutely dated tree-ring chronology. The data helped reveal a major solar proton event (SPE) which caused a spike in the production rate of cosmogenic radionuclides around 2610/2609 BP. This production event is thought to have reached a magnitude similar to the 774/775 AD production event but has remained undetected due to averaging effects in the decadal calibration data. The record leading up to the 2610/2609 BP event reveals a 11-yr solar cycle with varying cyclicity. Features of the new data and the benefits of higher resolution calibration are discussed.
Advances in accelerator mass spectrometry have resulted in an unprecedented amount of new high-precision radiocarbon (14C) -dates, some of which will redefine the international 14C calibration curves (IntCal and SHCal). Often these datasets are unaccompanied by detailed quality insurances in place at the laboratory, questioning whether the 14C structure is real, a result of a laboratory variation or measurement-scatter. A handful of intercomparison studies attempt to elucidate laboratory offsets but may fail to identify measurement-scatter and are often financially constrained. Here we introduce a protocol, called Quality Dating, implemented at ETH-Zürich to ensure reproducible and accurate high-precision 14C-dates. The protocol highlights the importance of the continuous measurements and evaluation of blanks, standards, references and replicates. This protocol is tested on an absolutely dated German Late Glacial tree-ring chronology, part of which is intercompared with the Curt Engelhorn-Center for Archaeometry, Mannheim, Germany (CEZA). The combined dataset contains 170 highly resolved, highly precise 14C-dates that supplement three decadal dates spanning 280 cal. years in IntCal, and provides detailed 14C structure for this interval.
Compound-specific radiocarbon (14C) dating often requires working with small samples of < 100 µg carbon (µgC). This makes the radiocarbon dates of biomarker compounds very sensitive to biases caused by extraneous carbon of unknown composition, a procedural blank, which is introduced to the samples during the steps necessary to prepare a sample for radiocarbon analysis by accelerator mass spectrometry (i.e., isolating single compounds from a heterogeneous mixture, combustion, gas purification and graphitization). Reporting accurate radiocarbon dates thus requires a correction for the procedural blank. We present our approach to assess the fraction modern carbon (F14C) and the mass of the procedural blanks introduced during the preparation procedures of lipid biomarkers (i.e. n-alkanoic acids) and lignin phenols. We isolated differently sized aliquots (6–151 µgC) of n-alkanoic acids and lignin phenols obtained from standard materials with known F14C values. Each compound class was extracted from two standard materials (one fossil, one modern) and purified using the same procedures as for natural samples of unknown F14C. There is an inverse linear relationship between the measured F14C values of the processed aliquots and their mass, which suggests constant contamination during processing of individual samples. We use Bayesian methods to fit linear regression lines between F14C and 1/mass for the fossil and modern standards. The intersection points of these lines are used to infer F14Cblank and mblank and their associated uncertainties. We estimate 4.88 ± 0.69 μgC of procedural blank with F14C of 0.714 ± 0.077 for n-alkanoic acids, and 0.90 ± 0.23 μgC of procedural blank with F14C of 0.813 ± 0.155 for lignin phenols. These F14Cblank and mblank can be used to correct AMS results of lipid and lignin samples by isotopic mass balance. This method may serve as a standardized procedure for blank assessment in small-scale radiocarbon analysis.
A new method to extract CO2 in seawater samples for the determination of F14C has been developed in the Laboratory of Ion Beam Physics at ETH Zurich. The setup consists of an automated sampler designed to extract dissolved inorganic carbon (DIC) from 7 samples in a row, by flushing the seawater with He gas to extract CO2. The fully automated method is controlled via a LabVIEW program that runs through all consecutive steps: catalyst preconditioning, CO2 extraction, CO2 trapping, thermal CO2 release from the trap into the reactor and finally the graphitization reaction which is performed simultaneously in the 7 reactors. The method was optimized by introducing a Cu-Ag furnace that was placed between the water and zeolite traps, which resulted in a better and faster graphitization performance (<2 hr) compared to previously used techniques. The method showed to be reproducible with an unprecedented precision of 1.7‰ even though consuming only 50–60 mL of seawater. The high throughput of 21 samples per day allows for coverage of future oceanographic transects with high spatial resolution, thus fostering the use of radiocarbon (14C) as water mass tracer.
The accelerator mass spectrometry (AMS) center at Horia Hulubei National Institute for R&D in Physics and Nuclear Engineering, Bucharest, is based on the latest-generation 1 MV Tandetron® accelerator, produced by High Voltage Engineering Europa (HVEE), The Netherlands. The AMS center became fully functional at the start of 2013, and at the end of 2015 the laboratory established the RoAMS international code and it was added to the list of AMS laboratories maintained by Radiocarbon journal. An important aspect in the establishment of a new AMS laboratory is the declaration and documentation of the adopted protocols and to demonstrate the reliability and reproducibility of the measurements in comparison to internationally recognized reference materials. In this paper, we present the dating results on the Sixth International Radiocarbon Intercomparison (SIRI) samples that were pretreated, graphitized, and measured in our laboratory. The newly developed sample preparation laboratory can handle sample materials as (1) organic materials, (2) wood, (3) bones, and (4) carbonates. The results of our measurements are in very good agreement with the SIRI consensus values and confirm the reliability of our sample preparation laboratory and also the good performance of the HVEE AMS system. The blank levels for the SIRI materials are 0.277±0.045/0.333±0.046 percent modern carbon (pMC) for wood samples, 0.441±0.038 pMC for bone collagen, and 0.239±0.030 pMC for carbonate materials, considering an average mass of 1 mg sample graphite.