• High-Precision Radiocarbon Dating of the Construction Phase of Oakbank Crannog, Loch Tay, Perthshire

      Cook, G. T.; Dixon, T. N.; Russell, N.; Naysmith, P.; Xu, S.; Andrian, B. (Department of Geosciences, The University of Arizona, 2010-01-01)
      Many of the Loch Tay crannogs were built in the Early Iron Age and so calibration of the radiocarbon ages produces very broad calendar age ranges due to the well-documented Hallstatt plateau in the calibration curve. However, the large oak timbers that were used in the construction of some of the crannogs potentially provide a means of improving the precision of the dating through subdividing them into decadal or subdecadal increments, dating them to high precision and wiggle-matching the resulting data to the master 14C calibration curve. We obtained a sample from 1 oak timber from Oakbank Crannog comprising 70 rings (Sample OB06 WMS 1, T103) including sapwood that was complete to the bark edge. The timber is situated on the northeast edge of the main living area of the crannog and as a large and strong oak pile would have been a useful support in more than 1 phase of occupation and may be related to the earliest construction phase of the site. This was sectioned into 5-yr increments and dated to a precision of approximately 8-16 14C yr (1 ). The wiggle-match predicts that the last ring dated was formed around 500 BC (maximum range of 520-465 BC) and should be taken as indicative of the likely time of construction of Oakbank Crannog. This is a considerable improvement on the estimates based on single 14C ages made on oak samples, which typically encompassed the period from around 800-400 BC.
    • Improved AMS 14C Dating of Shell Carbonates Using High-Precision X-Ray Diffraction and a Novel Density Separation Protocol (CarDS)

      Douka, K.; Hedges, R. E. M.; Higham, T. F. G. (Department of Geosciences, The University of Arizona, 2010-01-01)
      One critical variable in the successful application of radiocarbon dating is the effective removal of carbonaceous contaminants. In the case of marine carbonates, contamination appears usually in the form of secondary low-magnesium calcite, the stable polymorph of calcium carbonate and byproduct of the post-mortem recrystallization or replacement of the autochthonous phase, originally in the form of high-magnesium calcite or aragonite. Depending on the nature of the depositional environment, the secondary phase may be contemporary in age with the original shell carbonate and may have even been derived from it by dissolution-recrystallization processes, or can be an exogenous contaminant of younger or older age. The limited ability of current pretreatment protocols to detect and remove the secondary mineralogical phases prior to dating carbonates has been one of the reasons marine shell and coral 14C determinations are often difficult to validate in terms of their reliability. We have developed a new pretreatment protocol designed to achieve greater reliability and accuracy in the dating of this material. The method entails 2 steps. The first one involves the improved detection and quantification of secondary calcite in aragonite using X-ray diffraction, at a precision of ~0.1% and ~0.8%, respectively. Next, where this is required, a novel density separation step using non-toxic heavy liquids (CarDS) is applied to the diagenetic sample. This enables the clear separation of calcite and aragonite, with only the latter kept for dating. We have applied the new steps, screening and separation, on standard and archaeological examples and our initial results suggest that it is successful and reproducible. In this paper, we describe the method and initial results.
    • Improved Application of Bomb Carbon in Teeth for Forensic Investigation

      Wang, N.; Shen, C. D.; Ding, P.; Yi, W. X.; Sun, W. D.; Liu, K. X.; Ding, X. F.; Fu, D. P.; Yuan, J.; Yang, X. Y.; et al. (Department of Geosciences, The University of Arizona, 2010-01-01)
      While radiocarbon is widely applied in dating ancient samples, recent studies reveal that 14C concentrations in modern samples can also yield precise ages due to the atmospheric testing of thermonuclear devices between 1950 and 1963. 14C concentrations in both enamel and organic matter of 13 teeth from 2 areas in China were examined to evaluate and improve this method of forensic investigation. Choosing enamel near the cervix of the tooth can reduce the error caused by the difference between the sample formation time and whole enamel formation time because tooth enamel formations take a long time to complete. A proper regional data set will be helpful to get an accurate result when calculating the age of the sample (T1) by the CALIBomb program. By subtracting the enamel formation time (t), the birth date of an individual (T2) can be confirmed by enamel F14C from 2 teeth formed at different ages. Calculated enamel formation dates by 14C concentration are basically consistent with corresponding actual values, with a mean error of 1.9 yr for all results and 0.2 yr for the samples formed after AD 1960. This method is more effective for dating samples completed after AD 1960. We also found that 14C concentrations in organic matter of tooth roots are much lower than atmospheric concentrations in root formation years, suggesting that the organic material keeps turning over even after tooth formation is complete. This might be a potential tool for identification of death age to extract a proper component for 14C dating. We also observed that delta-13C values between hydroxyapatite and organic matter indicate that isotopic fractionation during the biomineralization is 8-9‰ more positive in mineral fractions than in organic matter.
    • Is More Precise Dating of Paleoindian Expansion Feasible?

      Fiedel, S. J.; Kuzmin, Y. V. (Department of Geosciences, The University of Arizona, 2010-01-01)
      Recent efforts to precisely date the florescence of the Clovis culture in North America have been hampered by both practical and theoretical problems: 1) The era of Clovis expansion (about 11,200-10,700 BP or 13,200-12,700 cal BP) coincides with the gap between the anchored central European tree-ring sequence (back to 12,400 cal BP) and the floating Bolling-Allerod sequence; 2) Clovis seems to immediately precede the onset of the Younger Dryas (YD) stadial. The "black mats" of the US Southwest appear to mark the regional occurrence of this climatic downturn. However, the timing and means of long-distance propagation of this climatic event are not yet well understood. Greenland ice cores (GISP2, GRIP, and NGRIP) remain poorly synchronized, with a discrepancy of 100 to 250 yr for the date of onset (as late as 12,700 cal BP, or as early as 12,950 cal BP); 3) The YD onset was accompanied by a rapid drop of radiocarbon ages from 11,000 to 10,600 BP in less than a century. The mechanism causing this was probably a change in overturning circulation in the North Atlantic. Do variable Clovis ages, often from what appear to be single-occupation contexts, reflect this "cliff" effect, slightly earlier minor reversals during the late Allerd, or simply the practical limitations of precision of the 14C method? 4) Dates for Fishtail or Fell I sites (with fluted, stemmed points) in southern South America are statistically indistinguishable from Clovis dates in North America. Does this imply very rapid population expansion, diffusion of tool-making techniques through long-established local populations (as argued by Waters and Stafford 2007), or abnormally large interhemispheric 14C offsets? 5) Are recent ostensibly high-precision collagen-derived dates for Paleoindian-associated fauna (e.g. horse and mammoth) reliable? Are interlaboratory blind tests of the new filtration processes necessary?
    • Laser-Heated Microfurnace: Gas Analysis and Graphite Morphology

      Smith, A. M.; Yang, B.; Hua, Q.; Mann, M. (Department of Geosciences, The University of Arizona, 2010-01-01)
      We describe progress in developing a novel miniaturized laser-heated 'microfurnace' aimed at preparing ultra-small (~5 g) graphite samples from CO2 (Smith et al. 2006, 2007, 2010). Recent effort has focused on automation of the process using a LabVIEW interface, which has permitted feedback control of the catalyst temperature as the reaction proceeds and the logging of reaction parameters. We trialed a number of different pure iron catalysts as well as Fe2O3 (which is reduced in situ to iron) and discuss the reaction rates. We studied the graphite morphology by scanning electron microscopy (SEM) and found there is a marked difference in graphite morphology with catalyst type. We assessed how each catalyst performs in the cesium sputter ion source of the ANTARES Accelerator Mass Spectrometry (AMS) facility. We utilized a quadrupole mass spectrometer to study the gas composition during the reaction, in order to better understand the underlying chemical reactions for such small samples and to better estimate the overall efficiency of the process. Results show that all CO2 is converted to CO by reduction on the iron catalyst within a few minutes of applying laser power. The reaction pressure stabilizes after 40 min; however, some CO is not converted to graphite. The cold trap temperature of -80 C is effective at trapping H2O, so there is little CH4 production.
    • Letter from the Editor

      Jull, A. J. T. (Department of Geosciences, The University of Arizona, 2010-01-01)
    • Measuring Submicron-Size Fractionated Particulate Matter on Aluminum Impactor Disks

      Buchholz, B. A.; Zermeño, P.; Wang, H-M.; Young, T. M.; Guilderson, T. P. (Department of Geosciences, The University of Arizona, 2010-01-01)
      Submicron-sized airborne particulate matter (PM) is not collected well on regular quartz or glass fiber filter papers. We used a micro-orifice uniform deposit impactor (MOUDI) to fractionate PM into 6 size fractions and deposit it on specially designed high-purity thin aluminum disks. The MOUDI separated PM into fractions 56-100, 100-180, 180-320, 320-560, 560-1000, and 1000-1800 nm. Since the MOUDI has a low flow rate (30 L/min), it takes several days to collect sufficient carbon on 47-mm foil disks. The small carbon mass (20-200 g C) and large aluminum substrate (~25 mg Al) present several challenges to production of graphite targets for accelerator mass spectrometry (AMS) analysis. The Al foil consumes large amounts of oxygen as it is heated and tends to melt into quartz combustion tubes, causing gas leaks. We describe sample processing techniques to reliably produce graphitic targets for 14C AMS analysis of PM deposited on Al impact foils.
    • MICADAS: Routine and High-Precision Radiocarbon Dating

      Wacker, L.; Bonani, G.; Friedrich, M.; Hajdas, I.; Kromer, B.; Němec, N.; Ruff, M.; Suter, M.; Synal, H.-A.; Vockenhuber, C. (Department of Geosciences, The University of Arizona, 2010-01-01)
      The prototype mini carbon dating system (MICADAS) at ETH Zurich has been in routine operation for almost 2 yr. Because of its simple and compact layout, setting up a radiocarbon measurement is fast and the system runs very reliably over days or even weeks without retuning. The stability of the instrument is responsible for the good performance in highest-precision measurements where results of single samples can be reproduced within less than 2. The measurements are described and the performance of MICADAS is demonstrated on measured data.
    • New Dating Evidence for North Sea Trade between England, Scotland, and Norway in the 11th Century AD

      Hall, D. W.; Cook, G. T.; Hamilton, W. D. (Department of Geosciences, The University of Arizona, 2010-01-01)
      This study follows on from previous research at Perth, Scotland, in which we dated carbonized food residues removed from the external surface of rim sherds of cooking pots of London Sandy Shellyware pottery (Museum of London Pottery Fabric Code SSW). The 15 residues that were dated produced 14C ages between 910 +/- 35 and 1085 +/- 40 BP. We have now carried out radiocarbon measurements on similar residues from the same fabric obtained from the Billingsgate excavations in London and the Bryggen excavations in Bergen, Norway. The London and Bergen measurements gave age ranges of 905 +/- 35 to 1115 +/- 35 BP and 920 +/- 35 to 1055 +/- 35 BP, respectively, both very similar to the Perth age range. The measurements at each site are in agreement with our Bayesian model assumption that they belong to a single phase of activity. The model estimates the introduction of London Sandy Shellyware in London to cal AD 820-1020, in Perth to cal AD 930-1020, and in Bergen to cal AD 980-1030 (95% probability). Further modeling predicts that it fell out of use in the reverse order.
    • Obituary: Austin Long

      Eastoe, C.; Leavitt, S.; Tanner Elliott, K.; Sewell, D. (Department of Geosciences, The University of Arizona, 2010-01-01)
    • Optimization of 236U AMS at CIRCE

      De Cesare, Y.; Quinto, F.; Sabbarese, C.; D, N.; D'Onofrio, A.; Alanella, L.; Petraglia, A.; Roca, V.; Terrasi, F. (Department of Geosciences, The University of Arizona, 2010-01-01)
      Actinide isotopes are present in environmental samples at ultra-trace levels (236U concentration is quoted to be on the order of pg/kg or fg/kg). Their detection requires the resolution of mass spectrometry (MS) techniques, but only accelerator mass spectrometry (AMS) has the sensitivity required. In order to perform the isotopic ratio measurements of actinides, such as 236U/238U, an upgrade of the Center for Isotopic Research on Cultural and Environmental Heritage accelerator (CIRCE) in Caserta, Italy, has been performed. The system was originally equipped for radiocarbon AMS measurements. The main difficulty of AMS measurement of 236U is the intense neighboring beam of 238U. Although most of the 238U ions are suppressed by means of magnetic and electrostatic elements, a small fraction of this intense beam can interfere with the rare isotopes. This paper reports the preliminary results of the 236U/238U isotopic ratio measurement limit 5.6 x 10^(-11)), aimed also to better understand the origin of background ions. For this purpose, a large 16-strip silicon detector providing spatial resolution has been used. In addition, calculations to assess the performance of the system obtained by adding a high-resolution time of flight-energy (TOF-E) detector are discussed.
    • Paleodiet Reconstruction of Human Remains from the Archaeological Site of Natfieh, Northern Jordan

      Al-Bashaireh, K.; Al-Shorman, A.; Rose, J.; Jull, A. J. T.; Hodgins, G. (Department of Geosciences, The University of Arizona, 2010-01-01)
      This investigation concerns human teeth and bones from the site of Natfieh, north Jordan. Nitrogen and carbon isotope analyses were used to model the paleo-economy by reconstructing Natfieh's paleodiet during a specific time period. 14C dating of human teeth and bones from the site of Natfieh, north Jordan, demonstrate that they belong to the Early Roman period and match the archaeological date from the tomb and grave goods typology. Stable isotope analyses of these humans have provided new information about the subsistence and society of individuals buried at Natfieh. Natfieh is today agriculturally productive and must have been so in antiquity with most of the foodstuffs having been produced locally. The long distance between Natfieh and the closest aquatic food source (Mediterranean Sea and Lake Tiberias) and the high cost of land transportation might be the reason for the low consumption of marine protein. The results agree with past research on the Roman diet showing that plants were the common source of food for the Romans and fish may have been restricted to elite members of the society.
    • Paleoenvironment of Medieval Archaeological Sites in Central Japan: Assemblage Analysis and 14C Dating of Insect Fossils

      Okuno, E.; Mori, Y.; Nakamura, T. (Department of Geosciences, The University of Arizona, 2010-01-01)
      This study aimed to investigate the paleoenvironment of 2 Medieval archaeological sites, Onigashioya and Ooke, in central Japan, by assemblage analyses of insect fossils preserved in sediments at the sites. In the Onigashioya site located in Mie Prefecture, the sclerites of insect fossils classified as the "village" type were detected, which indicates that human activities, and in particular farming, were taking place there. Rice paddies and fields existed near the site, which explains why many insects harmful to rice plants and crops were detected in the area. The radiocarbon date for sclerite remains of Hydrophilus acuminatus, an aquatic beetle that live in rice paddy fields, was calibrated to be cal AD 1010-1155. Analysis of sclerite remains of Craspedonotus tibialis, a ground beetle that typically inhabits seashore environments, resulted in a date of cal AD 1020-1155. This finding suggests that human settlements existed in the seaside areas of the Onigashioya site in the 11th century AD. In the Ooke site located in Aichi Prefecture, "insect pits" were found, which are structural remains containing a large number of Anomala rufocuprea, an insect that preys on field crops. Farmers would have gathered the insects from the fields and buried the dead remains in the pits. Accelerator mass spectrometry (AMS) 14C dates on sclerite remains of A. rufocuprea ranged from cal AD 1264 to 1385. It should be noted that fruit trees and vegetable crops were planted widely around the site in the 13th century AD. As the result, A. rufocuprea propagated greatly around the site in that period. It is probable that many insects harmful to field crops multiplied largely in this region due to the development of local woods and plains into farming fields. This type of development occurred throughout Japan during the Medieval period.
    • Personal Recollections of a Good Experiment

      Nelson, E. (Department of Geosciences, The University of Arizona, 2010-01-01)
    • Radiocarbon and Archaeology in Japan and Korea: What Has Changed because of the Yayoi Dating Controversy?

      Shoda, S. (Department of Geosciences, The University of Arizona, 2010-01-01)
      Since the sensational 2003 announcement that pushed the start of the Yayoi period back by 500 yr, archaeologists working on 1st millennium BC material from northeast Asia have had to switch from the older short chronology to a new long chronology. However, this change need not apply to the entire northeast Asian region as China's chronology is tied to written records. The timeline of the Korean peninsula, intermediate between the Chinese and Japanese ones, needs to be reexamined. The chronology of the 1st millennium BC in the Korean peninsula is still in dispute, in part because many of the radiocarbon dates lack clear archaeological contexts. This paper shows that a reliable typological relationship observed in archaeological materials existed at this time linking northeast Asia from China to Japan. This paper includes absolute dates based on the initial AMS 14C measurements of charred crops from South Korean sites.
    • Radiocarbon and Tritium Levels along the Romanian Lower Danube River

      Varlam, Carmen; Stefanescu, Ioan; Cuna, Stela; Vagner, Irina; Faurescu, Ionut; Faurescu, Denisa (Department of Geosciences, The University of Arizona, 2010-01-01)
      The Lower Danube Basin covers the Romanian-Bulgarian sub-basin downstream from Cazane Gorge and the sub-basins of the Siret and Prut rivers. To extensively survey the Romanian nuclear power plant impact on the Danube water, tritium and radiocarbon baseline values are required. Therefore, the reported study tried to establish these values based on a 2-yr sampling campaign covering 975 km of the Danube from Cazane Gorge to Tulcea. The tributaries Cerna, Jiu, Olt, and Arges were also included in this study. During the sampling campaigns, tritium concentration of different sampling locations showed values between 7 ± 2.1 and 33.5 ± 2.3 TU. Measured 14C activity for the same locations ranged between 88.45 ± 1.46 and 112.36 ± 1.56 pMC. Lower values were recorded for tributaries: between 8.3 ± 2.1 and 12.2 ± 2.2 TU for tritium and between 67.3 ± 1.29 and 86.04 ± 1.42 pMC for 14C. Despite the nuclear activity in the observed areas, tritium and 14C activities presented slightly higher values for specific locations without any influence on Danube River water.
    • Radiocarbon Chronology for Early Caves of the Mogao Grottoes at Dunhuang, China

      Qinglin, G.; Takabayashi, H.; Nakamura, T.; Gangquan, C.; Okada, K.; Bomin, S.; Yuquan, F.; Nishimoto, H. (Department of Geosciences, The University of Arizona, 2010-01-01)
      The Mogao Grottoes site at Dunhuang is one of the largest stone cave temples in China. The site features 735 caves with Buddhist mural paintings. To investigate the chronology of early caves of the Mogao Grottoes, radiocarbon dates were measured by accelerator mass spectrometry (AMS) on plant remains collected from 4 caves: 268, 272, 275, and 285. Caves 268, 272, and 275 are regarded (by archaeological analysis) to be the earliest existing caves in the Mogao Grottoes. The fourth cave, 285, features inscriptions on the north wall mentioning the oldest dates of the Chinese Mogao era. Plant materials, taken from the plaster layer of mural paintings and core materials from statues, were collected as samples (n = 11) for AMS 14C dating at Nagoya University. Two samples from cave 275 gave calibrated 14C ages of cal AD 380-430 (1 sigma). The other samples resulted in a time interval of cal AD 400-550. The calibrated 14C ages obtained for the samples taken from painted murals and the statues in cave 285 are consistent with the date given by the inscription remaining on the cave's north wall.
    • Radiocarbon Dates Documenting the Neolithic-Bronze Age Transition in Korea

      Kim, J. C.; Bae, C. J. (Department of Geosciences, The University of Arizona, 2010-01-01)
      We report radiocarbon dates for ~150 archaeological sites in Korea belonging to the Neolithic-Bronze Age transition period. From the present compilation, we find that the Neolithic-Bronze Age transition in Korea started as early as ~2300 BC and continued over the course of 800-900 yr with peaks representing population increases occurring 2-3 times. Compared with cases in other regions of the world, the Neolithic-Bronze Age transition in Korea was similar in both magnitude and transition time. However, the process in Korea appears to have occurred about 2000 yr later. Further, we find that the attempt to explain the Neolithic-Bronze Age transition in Korea as a migration hypothesis based only on a sudden population increase is not tenable.
    • Radiocarbon Dating of Individual Amino Acids from Archaeological Bone Collagen

      McCullagh, J. S. O.; Marom, A.; Hedges, R. E. M. (Department of Geosciences, The University of Arizona, 2010-01-01)
      Since the development of accelerator mass spectrometry (AMS) for radiocarbon dating in the late 1970s, its ability to date small samples of bone has been of huge importance in archaeology and Quaternary paleoecology. The conventional approach to sample preparation has been to extract and gelatinize protein, which is then combusted and graphitized for analysis. However, this 'bulk protein' can contain a heterogeneous mixture of non-collagenous molecules, including humic acids and other soil components that may be of a different age than the bone and therefore affect the accuracy of its 14C date. Sample pretreatment methods have been an important area of development in recent years but still show inadequacies for the dating of severely contaminated bone. The idea of isolating and dating individual compounds such as single amino acids, to improve dating accuracy, has been discussed in the literature since the 1960s. Hydroxyproline, for example, makes up over 10% of bone collagen but is extremely rare in most other animal proteins, increasing the chances of its presence being endogenous to the individual being dated. Its successful isolation has therefore been considered a potential 'gold standard' for dating archaeological bone; however, extracting and suitably purifying single amino acids from bone has proved a challenging task. This paper presents a novel method for the compound-specific 14C dating of individual amino acids, including hydroxyproline, from archaeological bone protein. It is based on a preparative, mixed-mode liquid chromatography separation of underivatized amino acids, entirely in aqueous solution and free of organic solvents. The method is presented here in detail including application to standard bone samples establishing its accuracy and background carbon contribution. Results from 14C dating hydroxyproline and other individual amino acids, from both historical and archaeological bone, are shown to provide AMS dates that are statistically indistinguishable from those of the bulk protein.
    • Radiocarbon Dating of Kohitsugire Calligraphies Attributed to Asukai Masatsune and the Periods of Origin of Genji Monogatari Emaki and Ban-dainagon Ekotoba

      Oda, H.; Ikeda, K. (Department of Geosciences, The University of Arizona, 2010-01-01)
      Genji monogatari emaki and Ban-dainagon ekotoba are Japanese national treasures. Although the periods in which they were painted have not been accurately determined, radiocarbon dating cannot be applied to these priceless artifacts because of the destructive nature of 14C dating. In this study, the periods of their origin were determined by 14C dating the kohitsugire calligraphy. Kohitsugire are ancient paper sheets containing graceful calligraphy. They originally were part of ancient manuscripts. Two kohitsugire named Imaki-gire and Kingin-kirihaku-wakanroeishu-gire are written in the same style as Genji monogatari emaki and Ban-dainagon ekotoba. Although Imaki-gire and Kingin-kirihaku-wakanroeishu-gire had been attributed to Asukai Masatsune (AD 1170-1221) on the basis of the kiwamefuda certificates, recent calligraphical and paleographical studies suggest that they are genuine handwritings of Fujiwara no Norinaga (AD 1109-1180). We applied 14C dating by accelerator mass spectrometry (AMS) to Imaki-gire and Kingin-kirihaku-wakanroeishu-gire. The calibrated 14C ages of both the kohitsugire indicated timing close to the peak of Fujiwara no Norinaga's career as a calligraphist. Based on the associations between the dated texts and the 14C results, it is concluded that the Genji monogatari emaki and Ban-dainagon ekotoba paintings could have been created in the middle of 12th century.