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Concept: Accelerator mass spectrometry

57

Tendons are often injured and heal poorly. Whether this is caused by a slow tissue turnover is unknown, since existing data provide diverging estimates of tendon protein half-life that range from 2 mo to 200 yr. With the purpose of determining life-long turnover of human tendon tissue, we used the (14)C bomb-pulse method. This method takes advantage of the dramatic increase in atmospheric levels of (14)C, produced by nuclear bomb tests in 1955-1963, which is reflected in all living organisms. Levels of (14)C were measured in 28 forensic samples of Achilles tendon core and 4 skeletal muscle samples (donor birth years 1945-1983) with accelerator mass spectrometry (AMS) and compared to known atmospheric levels to estimate tissue turnover. We found that Achilles tendon tissue retained levels of (14)C corresponding to atmospheric levels several decades before tissue sampling, demonstrating a very limited tissue turnover. The tendon concentrations of (14)C approximately reflected the atmospheric levels present during the first 17 yr of life, indicating that the tendon core is formed during height growth and is essentially not renewed thereafter. In contrast, (14)C levels in muscle indicated continuous turnover. Our observation provides a fundamental premise for understanding tendon function and pathology, and likely explains the poor regenerative capacity of tendon tissue.-Heinemeier, K. M., Schjerling, P., Heinemeier, J., Magnusson, S. P., Kjaer, M. Lack of tissue renewal in human adult Achilles tendon is revealed by nuclear bomb (14)C.

Concepts: Mass spectrometry, Biology, Tendon, Achilles tendon, Nuclear weapon, Tendons, Carbon-14, Accelerator mass spectrometry

42

The transition from the Middle Paleolithic (MP) to Upper Paleolithic (UP) is marked by the replacement of late Neandertals by modern humans in Europe between 50,000 and 40,000 y ago. Châtelperronian (CP) artifact assemblages found in central France and northern Spain date to this time period. So far, it is the only such assemblage type that has yielded Neandertal remains directly associated with UP style artifacts. CP assemblages also include body ornaments, otherwise virtually unknown in the Neandertal world. However, it has been argued that instead of the CP being manufactured by Neandertals, site formation processes and layer admixture resulted in the chance association of Neanderthal remains, CP assemblages, and body ornaments. Here, we report a series of accelerator mass spectrometry radiocarbon dates on ultrafiltered bone collagen extracted from 40 well-preserved bone fragments from the late Mousterian, CP, and Protoaurignacian layers at the Grotte du Renne site (at Arcy-sur-Cure, France). Our radiocarbon results are inconsistent with the admixture hypothesis. Further, we report a direct date on the Neandertal CP skeleton from Saint-Césaire (France). This date corroborates the assignment of CP assemblages to the latest Neandertals of western Europe. Importantly, our results establish that the production of body ornaments in the CP postdates the arrival of modern humans in neighboring regions of Europe. This new behavior could therefore have been the result of cultural diffusion from modern to Neandertal groups.

Concepts: Spain, Western Europe, Neanderthal, Pleistocene, Upper Paleolithic, Mousterian, Middle Paleolithic, Accelerator mass spectrometry

27

Accelerator mass spectrometry (AMS) is the ultimate technique for measuring rare isotopes in small samples. Biological and biomedical applications of (14)C-AMS (bio-(14)C-AMS) commenced in the early 1990s and are now widely used in many research fields including pharmacology, toxicology, food, and nutrition. For accurate, precise, and reproducible bio-(14)C-AMS analysis, the graphitization step in sample preparation is the most critical step. So, various sample preparation methods for a process called graphitization have been reported for specific applications. Catalytic graphitization using either a flame-sealed borosilicate tube or a septa-sealed vial is a popular sample preparation method for bio-(14)C-AMS. In this review, we introduce the AMS system, especially for bio-(14)C-AMS. In addition, we also review the graphitization method for bio-(14)C-AMS to promote further understanding and improvement of sample preparation for this technique. Examples of catalytic graphitization methods over the past two decades are described.

Concepts: Sample, Spectroscopy, Mass spectrometry, Accuracy and precision, 1990s, 1990s music groups, Accelerator mass spectrometry

24

Human-mediated biological exchange has had global social and ecological impacts. In sub-Saharan Africa, several domestic and commensal animals were introduced from Asia in the pre-modern period; however, the timing and nature of these introductions remain contentious. One model supports introduction to the eastern African coast after the mid-first millennium CE, while another posits introduction dating back to 3000 BCE. These distinct scenarios have implications for understanding the emergence of long-distance maritime connectivity, and the ecological and economic impacts of introduced species. Resolution of this longstanding debate requires new efforts, given the lack of well-dated fauna from high-precision excavations, and ambiguous osteomorphological identifications. We analysed faunal remains from 22 eastern African sites spanning a wide geographic and chronological range, and applied biomolecular techniques to confirm identifications of two Asian taxa: domestic chicken (Gallus gallus) and black rat (Rattus rattus). Our approach included ancient DNA (aDNA) analysis aided by BLAST-based bioinformatics, Zooarchaeology by Mass Spectrometry (ZooMS) collagen fingerprinting, and direct AMS (accelerator mass spectrometry) radiocarbon dating. Our results support a late, mid-first millennium CE introduction of these species. We discuss the implications of our findings for models of biological exchange, and emphasize the applicability of our approach to tropical areas with poor bone preservation.

Concepts: DNA, Mass spectrometry, Africa, Chicken, Southern Africa, Subregion, East Africa, Accelerator mass spectrometry

10

The recent establishment of a minimum age estimate of 39.9 ka for the origin of rock art in Sulawesi has challenged claims that Western Europe was the locus for the production of the world’s earliest art assemblages. Tantalising excavated evidence found across northern Australian suggests that Australia too contains a wealth of ancient art. However, the dating of rock art itself remains the greatest obstacle to be addressed if the significance of Australian assemblages are to be recognised on the world stage. A recent archaeological project in the northwest Kimberley trialled three dating techniques in order to establish chronological markers for the proposed, regional, relative stylistic sequence. Applications using optically-stimulated luminescence (OSL) provided nine minimum age estimates for fossilised mudwasp nests overlying a range of rock art styles, while Accelerator Mass Spectrometry radiocarbon (AMS 14C) results provided an additional four. Results confirm that at least one phase of the northwest Kimberley rock art assemblage is Pleistocene in origin. A complete motif located on the ceiling of a rockshelter returned a minimum age estimate of 16 ± 1 ka. Further, our results demonstrate the inherent problems in relying solely on stylistic classifications to order rock art assemblages into temporal sequences. An earlier than expected minimum age estimate for one style and a maximum age estimate for another together illustrate that the Holocene Kimberley rock art sequence is likely to be far more complex than generally accepted with different styles produced contemporaneously well into the last few millennia. It is evident that reliance on techniques that produce minimum age estimates means that many more dating programs will need to be undertaken before the stylistic sequence can be securely dated.

Concepts: Spectroscopy, Estimator, Mass spectrometry, Chronology, Mathematical analysis, Carbon-14, Accelerator mass spectrometry, Geologic time scale

8

Above-ground thermonuclear weapons testing from 1952 through 1962 nearly doubled the concentration of radiocarbon ((14)C) in the atmosphere. As a result, organic material formed during or after this period may be radiocarbon-dated using the abrupt rise and steady fall of the atmospheric (14)C concentration known as the bomb-curve. We test the accuracy of accelerator mass spectrometry radiocarbon dating of 29 herbivore and plant tissues collected on known dates between 1905 and 2008 in East Africa. Herbivore samples include teeth, tusks, soft tissue, hair, and horn. Tissues formed after 1955 are dated to within 0.3-1.3 y of formation, depending on the tissue type, whereas tissues older than ca. 1955 have high age uncertainties (>17 y) due to the Suess effect. (14)C dating of tissues has applications to stable isotope (paleo)ecology and wildlife forensics. We use data from 41 additional samples to determine growth rates of tusks, molars, and hair, which improve interpretations of serial stable isotope data for (paleo)ecological studies. (14)C dating can also be used to calculate the time interval represented in periodic histological structures in dental tissues (i.e., perikymata), which in turn may be used as chronometers in fossil teeth. Bomb-curve (14)C dating of confiscated animal tissues (e.g., ivory statues) can be used to determine whether trade of the item is legal, because many Convention of International Trade of Endangered Species restrictions are based on the age of the tissue, and thus can serve as a powerful forensic tool to combat illegal trade in animal parts.

Concepts: Mass spectrometry, Tissues, Atmosphere, Isotope, International trade, Radiocarbon dating, Carbon-14, Accelerator mass spectrometry

4

High-precision measurements of radiocarbon ((14)C) near or below a fraction modern 14C of one (F(14)C ≤ 1) are challenging and costly. An accurate, ultra-sensitive linear absorption approach to detecting (14)C would provide a simple and robust bench-top alternative to off-site accelerator mass spectrometry facilities. Here we report the quantitative measurement of (14)C in gas-phase samples of CO2 with F(14)C < 1 using cavity ring-down spectroscopy in the linear absorption regime. Repeated analysis of CO2 derived from the combustion of either biogenic or petrogenic sources revealed a robust ability to differentiate carbon samples with F(14)C < 1. With a combined uncertainty of (14)C/(12)C = 130 fmol/mol (F(14)C = 0.11), initial performance of the calibration-free instrument is sufficient to investigate a variety of applications in radiocarbon measurement science including the study of biofuels and bioplastics, illicitly traded specimens, bomb dating, and atmospheric transport.

Concepts: Spectroscopy, Oxygen, Mass spectrometry, Measurement, Metrology, Carbon, Carbon-14, Accelerator mass spectrometry

4

Methodological developments and new paleoanthropological data remain jointly central to clarifying the timing and systemic interrelationships between the Middle-Upper Paleolithic (MP-UP) archaeological transition and the broadly contemporaneous anatomically modern human-archaic biological turnover. In the recently discovered cave site of Mughr el-Hamamah, Jordan, in situ flint artifacts comprise a diagnostic early Upper Paleolithic (EUP) assemblage. Unusually well-preserved charcoal from hearths and other anthropogenic features associated with the lithic material were subjected to acid-base-wet oxidation-stepped combustion (ABOx-SC) pretreatment. This article presents the ABOx-SC accelerator mass spectrometry (AMS) radiocarbon dates on nine charcoal specimens from a single palimpsest occupation layer. Date calibration was carried out using the INTCAL13 radiocarbon calibration dataset. With the bulk of the material dating to 45-39 ka cal BP (thousands of years calibrated before present), the Mughr el-Hamamah lithic artifacts reveal important differences from penecontemporaneous sites in the region, documenting greater technological variability than previously known for this time frame in the Levant. The radiocarbon data from this EUP archaeological context highlight remaining challenges for increasing chronological precision in documenting the MP-UP transition.

Concepts: Time, Mass spectrometry, Jordan, Stone Age, Iraq, Prehistory, Radiocarbon dating, Accelerator mass spectrometry

2

The presence of tramadol in roots of Sarcocephalus latifolius trees in Northern Cameroon was recently attributed to point contamination with the synthetic compound. The synthetic origin of tramadol in the environment has now been unambiguously confirmed. Tramadol samples isolated from tramadol pills bought at a street market in downtown Maroua and highly contaminated soil at Houdouvou were analyzed by high-precision (14) C measurements by accelerator mass spectrometry ((14) C AMS): Tramadol from the pills did not contain any radiocarbon, thus indicating that it had been synthesized from (14) C-free petroleum-derived precursors. Crucially, tramadol isolated from the soil was also radiocarbon-free. As all biosynthetic plant compounds must contain radiocarbon levels close to that of the contemporary environment, these results thus confirm that tramadol isolated from the soil cannot be plant-derived. Analyses of S. latifolius seeds, in vitro grown plants, plants from different origins, and stable-isotope labeling experiments further confirmed that synthetic tramadol contaminates the environment.

Concepts: Spectroscopy, Mass spectrometry, Plant, Pollution, Root, Perennial plant, Carbon-14, Accelerator mass spectrometry

1

For radiocarbon results to be accurate, samples must be free of contaminating carbon. Sample pre-treatment using an HPLC approach has been developed at the Oxford Radiocarbon Accelerator Unit (ORAU) as an alternative to conventional methods for dating heavily contaminated bones. This approach isolates hydroxyproline from bone collagen, enabling a purified bone-specific fraction to then be radiocarbon dated by accelerator mass spectrometry (AMS).

Concepts: Sample, Spectroscopy, Bone, Mass spectrometry, Collagen, Connective tissue, Carbon-14, Accelerator mass spectrometry