Worldwide, dating rock art is difficult to achieve because of the frequent lack of datable material and the difficulty of removing contamination from samples. Our research aimed to select the paints that would be the most likely to be successfully radiocarbon dated and to estimate the quantity of paint needed depending on the nature of the paint and the weathering and alteration products associated with it. To achieve this aim, a two-step sampling strategy, coupled with a multi-instrument characterization (including SEM-EDS, Raman spectroscopy, and FTIR spectroscopy analysis) and a modified acid-base-acid (ABA) pretreatment, was created. In total, 41 samples were dated from 14 sites in three separate regions of southern Africa. These novel protocols ensure that the 14C chronology produced was robust and could also be subsequently applied to different regions with possible variations in paint preparation, geology, weathering conditions, and contaminants.

Bone remains of small vertebrate fossils provide valuable information for paleoenvironmental and paleoclimatic reconstructions. However, direct radiocarbon dating of small vertebrates remains challenging as the extraction of sufficient good quality collagen is required. The efficiency of eight collagen extraction protocols was tested on seven samples, representative of different ages and burial environments, including both macro and small vertebrate taxa. First, the samples were prescreened using attenuated total reflectance–Fourier transform infrared spectroscopy (ATR-FTIR) to quantify collagen content in archaeological bones, revealing that one should be discarded for 14C dating. Then, the quantity of protein extracted (yield) and collagen integrity were checked using conventional elemental analysis. The results show that one protocol was not able to accurately extract collagen from the samples. A soft HCl-based protocol seems more appropriate for the pretreatment of archaeological small mammal bones, whereas a harsher protocol might be more efficient to extract a higher amount of collagen from large mammals as well as amphibian bones. The influence of the tested protocols on carbon and nitrogen isotope values was also investigated. The results showed that isotopic variability, when existing, is related to the interindividual differences rather than the different protocols.

The A.E. Lalonde accelerator mass spectrometer (3MV, HVEE) was commissioned in early 2014 at the University of Ottawa (Canada). The radiocarbon sample preparation laboratory spent the better part of 2014 undertaking a quality control program, establishing pretreatment protocols, and streamlining sample processing. In the fall of 2014, the first unknown samples were accepted and in the first year of operation well over 1000 targets (~60% unknowns) were analyzed. Here, we present an overview of sample processing protocols and results from routinely measured standards, reference, and blank materials.

The sealed tube Zn reduction method has been applied for small-mass samples ranging from 15 to 100 μg carbon preparation for accelerator mass spectrometry (AMS) radiocarbon (14C) measurements at the AMS-14C Preparation Lab in Guangzhou Institute of Geochemistry, Chinese Academy of Sciences (GIGCAS). The volume of the sealed reactor tube is reduced to ~0.75 cm3 in order to increase the yield of graphite. Graphite targets are measured at the Keck Carbon Cycle AMS Facility at the University of California, Irvine (KCCAMS). The targets generate a maximum 12C+1 current of about 0.5 μA per 1 μg C. The modern-carbon background is estimated to be 0.25–0.60 μg C, and dead-carbon background to be ~0.3–0.9 μg C. Both modern-carbon background and dead-carbon background are size dependent, so the results can be corrected. The precision of the small-mass modern carbon standard samples is±15–25‰ for the size of ~15–20 μg C,±5–10‰ for ~20–50 μg C, and±3–10‰ for 50–100 μg C. Further reduction of dead-carbon and modern-carbon contamination is needed in preparation of small-mass samples at GIGCAS.

The main objective of this report is to present the dating process routinely applied to different types of samples at the Laboratoire de Mesure du Carbone 14 (LMC14). All the results and protocols refer to our procedures over the last 5 years. A description of the sorting and chemical pretreatments of the samples as well as the extraction and graphitization of CO2 are reported. Our last study concerning the degradation of the blank level according to the storage time of the targets between graphitization and accelerator mass spectrometry (AMS) measurement is also presented. This article also provides information on how to submit a valid laboratory sample. We give details relating to sampling procedures on site as well as contamination issues relative to the 14C dating methodology.

From the early days of radiocarbon dating, the standard sample treatment has involved removal of contamination from carbonates and humic acids by washes in acid and base, respectively. A modification of this acid-base-acid (ABA) method has been suggested, especially for material older than 20,000 yr. However, the criticism of ABA and application of a more aggressive oxidizing method, such as wet oxidation (ABOX) or cellulose extraction, might only be needed in some special cases, for example, in the case of poorly preserved or chemically treated wood. Separation of cellulose seems to be the ultimate solution; however, it is not always applicable when samples contain small amounts of wood. As a part of studies focusing on the chronology of late Pleistocene sedimentary processes in the Venetian–Friulian Plain and Carnic Alps (NE Italy), 14C analyses were performed on old wood samples found in sedimentary deposits of pre-Last Glacial Maximum (LGM) age. Wood samples were treated by five methods: ABA, two modified ABA treatments (ABOX and ABA+Bleach), as well as two different cellulose separations. Infrared spectra of treated samples and 14C results show that in most cases the ABA method is sufficient in removing the contamination of naturally deposited wood, even when the wood is of very old age.

We investigated age estimation of persons using 45 Japanese human teeth that consisted of mainly the third molar. We measured the radiocarbon content in tooth enamel hydroxyapatite from the crown as well as those in collagen and bioapatite in the root of the same tooth. Age estimations from tooth enamel apatite yielded an absolute age shift of 1.7±1.4 yr from the true age. This value suggests that estimating the age of Japanese people from tooth enamel is as accurate as the previous studies conducted in Europe and the USA. The 14C analysis of roots suggested that bioapatite is formed slightly later than collagen in the same tooth roots. The appropriate formation age ranges suggested by the tooth enamel analysis can be optimized and confirmed by using the additional F14C values of the root samples. We also noticed a characteristic trend of enamel δ13C values in comparison with the formation ages of the crowns of the teeth. The δ13C value tends to increase gradually from –13.0‰ to –11.5‰ from the 1960s to the 1970s, probably being caused by changes in the Japanese diet. This trend may support the selection of proper tooth formation age as supplemental data in addition to 14C content analyses.

At INFN-LABEC (Florence, Italy), a new pretreatment for radiocarbon dating based on chloroform has been recently set up. This method aims to remove the synthetic resins used for artwork restoration, which otherwise could alter the original 14C content. The present study characterizes the efficiency of the process when applied to wood. We have verified whether the effectiveness of the pretreatment depends on the number of extractions in chloroform. We prepared samples by applying different volumes of Paraloid B-72®, one of the most widespread products used in restoration, on poplar wood of known age. Contaminated samples were artificially aged in a climatic chamber. A fraction from each sample was collected before any treatment and after respectively 1, 2, 3, and 4 extractions in chloroform, and 14C dating by AMS, the resin appears to be already removed after the first two extractions. Furthermore, the extracted mixtures of chloroform and possible removed Paraloid were measured by FTIR spectroscopy, the results of which confirmed the 14C results. The efficiency of the pretreatment was also verified on historical wooden materials that had been previously restored. In these cases, a higher number of extractions is required, suggesting a careful approach when dealing with “real” artworks.

This study evaluates the radiocarbon dating of ceramic samples from Tupiguarani sites in Brazil, a settlement type dating up to 3000 cal BP. In this work, residues from ceramic samples from four archaeological sites in Rio de Janeiro (Morro Grande, Serrano, Barba Couto, and Bananeiras) were analyzed. In order to identify the most suitable sample preparation protocols, the humic fraction was isolated from the bulk material at the Oxford Radiocarbon Accelerator Unit (ORAU), whereas the acid-base-acid (ABA) residue fraction method was applied at the Radiocarbon Laboratory of the Fluminense Federal University (LAC-UFF). The dating results were compared to the current knowledge about the occupational periods of the sites. For the Morro Grande site, the results of humic and ABA residue fractions show a difference of more than 1500 yr. For the Serrano site, the 14C ages obtained from the two pretreatments are identical, and as with the Barba Couto and Bananeiras sites, indicate an occupation during the Brazilian colonial period of the 16th century AD and are compatible with the archaeological data.

The Dangoor REsearch Accelerator Mass Spectrometer (D-REAMS) is a dedicated carbon-only AMS system, built by National Electrostatics Corporation (NEC). It is based on the 1.5SDH Pelletron, operating at 460 keV. The machine was installed at the Weizmann Institute of Science, Rehovot, Israel, in January–February 2013, and passed the acceptance test on March 2013. Since then, over 4500 samples have been successfully measured. Here, we present the results of an intercomparison experiment, done in collaboration with the Vienna Environmental Research Accelerator (VERA), and some typical operation parameters and measurement values of the new AMS system.

Over the last few decades, radiocarbon laboratories have used different procedures for measuring a broad range of carbonaceous materials. To produce reliable results, the processes employed for sample processing, graphite target production, and spectrometer measurement must be rigorous, well tested, and reproducible. Most of the procedures have been developed, improved, and published as part of the laboratories’ quality control and research programs, and can be frequently found in the literature. Nevertheless, there are suites of laboratory techniques (or “small useful skills”), products, and other resources that either have never been described in publications, or have been somewhat hidden in much larger scientific articles and reports. We feel that with the rapid rise of newer laboratories and facilities, a set of resourceful suggestions might come in handy. Here we gathered these skill sets that can be used in all aspects of 14C sample processing, with the intention to simplify and expedite procedures, from glass-tube making to graphitization and measurements. We also included some miscellaneous items to help in laboratory setup.

Systematic investigations and experience from several application projects on small carbon samples over a number of years have resulted in measuring the radiocarbon content of 10 μg C samples with an overall precision of typically 1%. A substantial reduction of the carbon contamination during graphitization was achieved, resulting in 31±30 ng modern and <100 ng 14C-free carbon. Thus, graphitization is no longer the limiting factor because earlier sample preparation steps usually introduce much larger contamination. The method has been extended to a variety of materials and applied to various projects. Realistic conditions for procedure development can only be achieved in the context of applications on true samples; methods developed are the lyophilization of samples in solution, combustion, ultraviolet oxidation, or carbonate hydrolysis with phosphoric acid, which allows to prepare samples for a wide range of applications. Insights gained from systematic investigations and from real applications are presented.

The different categories of samples and their treatments at the radiocarbon (14C) laboratory in Jena, Germany, are described. The Jena 14C laboratory is dedicated to studying the global carbon cycle through the analysis of soil, plant, gas, charcoal, and wood samples. The respective preparation procedures for different samples types are presented, including wet-chemistry pretreatments for soil decalcification, charcoal purification using an acid–base–oxidation procedure (ABOx), and α-cellulose extraction from wood and leaves. In particular, investigations of the background corrections for each sample type are emphasized. Furthermore, an investigation of the contamination resulting from the storage of graphite is presented. Four storage conditions are investigated for storage times up to 30 months.

The Laboratory for the Analysis of Radiocarbon with AMS (LARA) was established at the University of Bern in 2013. Since then, the quality of sample preparation and radiocarbon measurement procedures have been validated for different materials such as plant remains, macrofossils, bulk sediment, charcoals, and wood. This article presents the optimization of sample pretreatment of bones based on protocols described in the literature. The extraction of collagen was performed with an acid-base-acid treatment, gelatinization, coarse filtration, lyophilization, and graphitization. Dating results were validated as satisfactory for the Holocene by investigation of 36 individual samples previously dated by other 14C laboratories including VIRI/SIRI materials and from well-known archaeological contexts. An additional blank contribution for bone treatment was determined by comparison with the preparation of other sample materials. The cases of two outliers from the Holocene were studied in detail.

The standard procedure for storing/preserving seawater dissolved organic carbon (DOC) samples after field collection is by freezing (–20°C) until future analysis can be made. However, shipping and receiving large numbers of these samples without thawing presents a significant logistical problem and large monetary expense. Access to freezers can also be limited in remote field locations. We therefore test an alternative method of preserving and storing samples for the measurement of DOC concentrations ([DOC]), stable carbon (δ13C), and radiocarbon (as ∆14C) isotopic values via UV photooxidation (UVox). We report a total analytical reproducibility of frozen DOC samples to be [DOC]±1.3 µM, ∆14C±9.4‰, and δ13C±0.1‰, comparable to previously reported results (Druffel et al. 2013). Open Ocean DOC frozen versus acidified duplicates were on average offset by ∆DOC±1.1 µM, ∆∆14C± –1.3‰, and ∆δ13C± –0.1‰. Coastal Ocean frozen vs. acidified sample replicates, collected as part of a long-term (380-day) storage experiment, had larger, albeit consistent offsets of ∆DOC±2.2 µM, ∆∆14C±1.5‰, and ∆δ13C± –0.2‰. A simple isotopic mass balance of changes in [DOC], ∆14C, and δ13C values reveals loss of semi-labile DOC (2.2±0.6 µM, ∆14C=–94±105‰, δ13C=–27±10‰; n=4) and semi-recalcitrant DOC (2.4±0.7 µM, ∆14C=–478±116‰, δ13C=–23.4±3.0‰; n=3) in Coastal and Open Ocean acidified samples, respectively.

A new type of miniaturized, externally heated graphitization reaction furnace, the microconventional furnace (MCF), was constructed following our development of the laser heated furnace (LHF). The MCF is comprised of a gas reactor, a cold finger cooling system, and a compact resistive heater, which can raise the temperature of the hot finger to 850°C. The gas reactor is provided with three integrated valves to connect with the hydrogen/vacuum manifold, to isolate the reactor, and to connect with sample vessels. We made two types of MCF: the type 1 furnace (volume of 0.9 mL), with an integral stainless steel cold finger, and the type 2 furnace (volume from 1.3 to 10 mL), with a changeable glass cold finger. The MCF is designed for above atmospheric pressure (up to 2500 mbar) operation to decrease the overall graphitization time and improve the carbon yield. The MCF provides an effective solution for producing graphite from carbon dioxide (CO2) sample gas from 5 to 2000 µg of carbon with only 0.083 μg of 100 pMC extraneous carbon added. Cross-contamination tests show that the MCFs have no memory effect from previous samples.

Combining atmospheric Δ14CO2 data sets from different networks or laboratories requires secure knowledge on their compatibility. In the present study, we compare Δ14CO2 results from the Heidelberg low-level counting (LLC) laboratory to 12 international accelerator mass spectrometry (AMS) laboratories using distributed aliquots of five pure CO2 samples. The averaged result of the LLC laboratory has a measurement bias of –0.3±0.5‰ with respect to the consensus value of the AMS laboratories for the investigated atmospheric Δ14C range of 9.6 to 40.4‰. Thus, the LLC measurements on average are not significantly different from the AMS laboratories, and the most likely measurement bias is smaller than the World Meteorological Organization (WMO) interlaboratory compatibility goal for Δ14CO2 of 0.5‰. The number of intercomparison samples was, however, too small to determine whether the measurement biases of the individual AMS laboratories fulfilled the WMO goal.

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.

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.