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In two forensic cases, radiocarbon (14C) bomb-pulse datings of human bones have been performed and analyzed using detailed models to correct for collagen-carbon turnover rates and reservoir effects. The modeled corrections are discussed and the resulting 14C ages compared to later information on actual time of birth and death of the individuals. Simple time lag corrections of bone dates are found to be inadequate, whereas modeling based on age dependent turnover rates and bomb-pulse levels through life combined with substantial reservoir age corrections can explain the observed 14C results.
When sampling mortars for radiocarbon (14C) dating it is crucial to ensure that the sample has hardened rapidly relative the resolution of the dating method. Soft and porous lime mortars usually fulfill this criterion if the samples are taken from an uncovered surface from less than a few centimeters deep. However, hard, concrete-like mortars may be impermeable for carbon dioxide and even the outermost centimeters may still contain uncarbonated calcium hydroxide. These mortars may harden very slowly and contain carbonate that formed centuries or even millennia after the original building phase, and they can still be alkaline and capture modern 14C, causing younger 14C ages than the actual construction age. Another problem is reactivation of the binder carbonate if it has been partly decarbonated during a fire later on in its history. It will be shown that these young carbonates dissolve rapidly in phosphoric acid and in many cases a reasonable 14C age can be read from 14C profiles in sequential dissolution if the measurements from initially formed carbon dioxide are disregarded. However, if a mortar was made waterproof deliberately by adding crushed or ground tile, as in Roman cocciopesto mortars, it may be very difficult to get a conclusive dating.
Lime lumps and bulk mortars show different 14C contamination when analyzed in several CO2 fractions isolated from the effervescence of an ongoing hydrolysis reaction. Age profiles of both materials are therefore highly complementary and together they can provide a reliable date. Furthermore, they can also reveal the complexity of the radiocarbon (14C) distribution within the mortar and thus prevent over-interpretation of the data. The lime lump versus bulk mortar dating data presented here has been collected over 22 years, with only a small fraction of the results so far published internationally. Since there has been an increasing interest in mortar dating over recent years with a special focus on lime lumps, and since many laboratories have just begun mortar dating experiments, we wish to present some of the extensive data that already exist. Previously published data from 15 lime lumps (including 34 14C measurements from sequential dissolution) and 43 new 14C measurements from 17 lime lumps are presented here. The samples are from medieval Finland and Sweden, classical Rome and medieval Italy, and the Roman Jerash (Gerasa), Jordan.
Absolute dating of mortars is crucial when trying to pin down construction phases of archaeological sites and historic stone buildings to a certain point in time or to confirm, but possibly also challenge, existing chronologies. To evaluate various sample preparation methods for radiocarbon (14C) dating of mortars as well as to compare different dating methods, i.e. 14C and optically stimulated luminescence (OSL), a mortar dating intercomparison study (MODIS) was set up, exploring existing limits and needs for further research. Four mortar samples were selected and distributed among the participating laboratories: one of which was expected not to present any problem related to the sample preparation methodologies for anthropogenic lime extraction, whereas all others addressed specific known sample preparation issues. Data obtained from the various mortar dating approaches are evaluated relative to the historical framework of the mortar samples and any deviation observed is contextualized to the composition and specific mineralogy of the sampled material.
Seven radiocarbon laboratories: Åbo/Aarhus, CIRCE, CIRCe, ETHZ, Poznań, RICH, and Milano-Bicocca performed separation of carbonaceous fractions suitable for 14C dating of four mortar samples selected for the MOrtar Dating Inter-comparison Study (MODIS). In addition, optically stimulated luminescence (OSL) analyses were completed by Milano-Bicocca and IRAMAT-CRP2A Bordeaux. Each laboratory performed separation according to laboratory protocol. Results of this first intercomparison show that even though consistent 14C ages were obtained by different laboratories, two mortars yielded ages different than expected from the archaeological context.
Marine records from the Reykjanes Ridge indicate ice sheet variations and abrupt climate changes. One of these records, ice-rafted detritus (IRD), serves as a proxy for iceberg discharges that probably indicates ice sheet fluctuations. The IRD records suggest that iceberg discharge 68,000–10,000 yr B.P. happened more frequently than the 7000- to 10,000-yr spacing of the Heinrich events. An IRD peak 67,000 to 63,000 yr B.P. further suggests that the Middle Weichselian glaciation started about 12,000 yr earlier in the North Atlantic than in the Norwegian Sea. Several later IRD events, in contrast, correlate with Norwegian Sea IRD-rich layers and imply coeval ice sheet advances in the North Atlantic and the Norwegian Sea. Coccoliths in a core from the Reykjanes Ridge show distinct peaks in species that record occasional inflow of warm surface water during the last glaciation, as previously reported from the eastern Labrador Sea. High abundances of coccoliths, together with a decrease of Neogloboquadrina pachyderma sin. and relatively low δ18O values, imply enhanced advection of the North Atlantic Current 69,000–67,000 yr B.P., 56,000–54,000 yr B.P., 35,000–33,000 yr B.P., and 26,000–23,000 yr B.P. This advection provided a regional moisture source for extension of ice sheets onto the shelf. In contrast, most of the IRD events are characterized by cold polar surface water masses indicating rapid variations in ocean surface conditions.
Cores and exposed cliff sections in salt marshes around Ho Bugt, a tidal embayment in the northernmost part of the Danish Wadden Sea, were subjected to 14C dating and litho- and biostratigraphical analyses to reconstruct paleoenvironmental changes and to establish a late Holocene relative sea-level history. Four stages in the late Holocene development of Ho Bugt can be identified: (1) groundwater-table rise and growth of basal peat (from at least 2300 BC to AD 0); (2) salt-marsh formation (0 to AD 250); (3) a freshening phase (AD 250 to AD 1600?), culminating in the drying out of the marshes and producing a distinct black horizon followed by an aeolian phase with sand deposition; and (4) renewed salt-marsh deposition (AD 1600? to present). From 16 calibrated AMS radiocarbon ages on fossil plant fragments and 4 calibrated conventional radiocarbon ages on peat, we reconstructed a local relative sea-level history that shows a steady sea-level rise of 4 m since 4000 cal yr BP. Contrary to suggestions made in the literature, the relative sea-level record of Ho Bugt does not contain a late Holocene highstand. Relative sea-level changes at Ho Bugt are controlled by glacio-isostatic subsidence and can be duplicated by a glacial isostatic adjustment model in which no water is added to the world's oceans after ca. 5000 cal yr BP.
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.
The settlement time of Iceland has been debated for years as radiocarbon dates of bulk wood samples have been interpreted to set a timing 150–200 yr earlier than indicated by tephrochronology (later than AD 871±2) and the Sagas (AD 874). This early date is also in conflict with the dating results on extensive series of short-lived material such as grain and domestic animal and human bone remains of early settlers. The old-wood effect for the charcoal and bulk wood samples has been suggested to explain this controversy. This study uses a Bayesian model, implemented in the OxCal program, to show that the charcoal data combined with short-lived material (grain/bone) suggest ages anywhere in the interval AD 854–922 (95.4% probability), indicating that the available 14C data cannot be taken as compelling evidence that there was a settlement any earlier than AD 922. The Bayesian model shows that the observed exponential distribution of the excess age of the bulk wood samples is exactly as expected if there was an old-wood effect evident in the samples.
Cherubini et al. (above) question the reliability of identifying annual growth increments in olive trees, and therefore voice caution against the result of the wiggle-match of the four sections of a branch of an olive tree to the 14C calibration curve. Friedrich et al. (2006) were well aware of the problematic density structure of olive trees, and therefore assigned rather wide error margins of up to 50 per cent to the ring count. This still resulted in a late seventeenth century BC youngest date for the modelled age range of the outermost section of wood (95.4% probability). One can even remove any constraint from ring counting altogether and model the four radial sections as a simple ordered sequence, in which only the relative position is used as prior information, in other words that outer sections are younger than inner ones in a radial section.
Since 1994, our team has gained extensive experience applying accelerator mass spectrometry (AMS) radiocarbon analysis for mortar dating, totaling over 465 samples and 1800+ measured CO2 fractions. Several samples have been analyzed repeatedly. The research covers both Medieval and Classical archaeology. We therefore believe our experience can be helpful when developing preparation procedures for different kinds of mortars in different areas and in varying chronologies. So far, the main areas of interest have been (a) the churches of the Åland Islands (in the archipelago between Finland and Sweden); (b) the churches in the Åboland Archipelago (SW Finland); (c) sites in the Iberian Peninsula including Torre de Palma (a Roman village in Portugal); and (d) Rome, Pompeii, and Herculaneum (Italy). Most of the analyses before 2000 were hydrolized in only two CO2 fractions per sample, and reliability criteria were defined on the basis of how well the ages of the two fractions agree with each other. These criteria have proved most helpful in determining the reliability of 14C mortar analyses. Different types of mortar have been investigated, including lime mortars made both from limestone and marble, pozzolana mortars, fire-damaged mortars, and mortars based on burnt shells. Most importantly, separate lime lumps sampled from these mortars have been analyzed sporadically and recently more systematically. The research also includes different types of hydrolysis applied in the pretreatment. In addition to using 85% phosphoric acid (H3PO4), the experimental research includes tests with smaller concentrations of phosphoric acid, and tests based on 2–3% hydrochloric acid (HCl) dissolutions. To characterize the dissolution process, results are presented as age profiles of 2–5 CO2 fractions. In our experience, pozzolana mortars have been difficult to date, and HCl dissolution should be used only in special cases and in complementary tests.
AMS-bascd radiocarbon dating was applied to Medieval lime mortars made from burned shells and aggregate including both shore sediments and neovolcanic rocks. Three mortar samples from the city of Leiden near Amsterdam were prepared using the same kind of acid hydrolysis technique as has been earlier used for dating mortars made from burned marble and limestone. Five consecutive CO2 fractions were collected from each sample to form age profiles as functions of the dissolution progress index. One of the samples, from a brick wall of known age, was taken as a reference from the Pieterskerk church. Two other samples were taken from the Burcht circular stronghold on a former island on the Rhine River. The age of Burcht is less well known; thus, the presented results are a contribution to an ongoing discussion on its history.
The freshwater reservoir effect is a potential problem when radiocarbon dating fish bones, shells, human bones, or food crusts on pottery from sites near rivers or lakes. The reservoir age in hardwater rivers can be up to several thousand years and may be highly variable. Accurate 14C dating of freshwater-based samples requires knowing the order of magnitude of the reservoir effect and its degree of variability. Measurements on modern riverine materials may not give a single reservoir age correction that can be applied to archaeological samples, but they show the order of magnitude and variability that can also be expected for the past. This knowledge will be applied to the dating of food crusts on pottery from the Mesolithic sites Kayhude at the Alster River and Schlamersdorf at the Trave River, both in Schleswig-Holstein, northern Germany.
Marine radiocarbon bomb-pulse time histories of annually resolved archives from temperate regions have been underexploited. We present here series of Δ14C excess from known-age annual increments of the long-lived bivalve mollusk Arctica islandica from 4 sites across the coastal North Atlantic (German Bight, North Sea; Troms⊘, north Norway; Siglufjordur, north Icelandic shelf; Grimsey, north Icelandic shelf) combined with published series from Georges Bank and Sable Bank (NW Atlantic) and the Oyster Ground (North Sea). The atmospheric bomb pulse is shown to be a step-function whose response in the marine environment is immediate but of smaller amplitude and which has a longer decay time as a result of the much larger marine carbon reservoir. Attenuation is determined by the regional hydrographic setting of the sites, vertical mixing, processes controlling the isotopic exchange of 14C at the air-sea boundary, 14C content of the freshwater flux, primary productivity, and the residence time of organic matter in the sediment mixed layer. The inventories form a sequence from high magnitude-early peak (German Bight) to low magnitude-late peak (Grimsey). All series show a rapid response to the increase in atmospheric Δ14C excess but a slow response to the subsequent decline resulting from the succession of rapid isotopic air-sea exchange followed by the more gradual isotopic equilibration in the mixed layer due to the variable marine carbon reservoir and incorporation of organic carbon from the sediment mixed layer. The data constitute calibration scries for the use of the bomb pulse as a high-resolution dating tool in the marine environment and as a tracer of coastal ocean water masses.
This study focuses on radiocarbon dating of mortars that have withstood city fires and display visible fire damage effects. Some fire-damaged and undamaged original Medieval mortars from the same site have also been tested. The mortars were heated at different temperatures and then analyzed using the same preparation procedures as in 14C dating of mortars to see what kind of changes the heating would introduce to the mineralogy, chemistry, and the carbon and oxygen isotope ratios. We found that decarbonation during heating starts at ∼600 ° and recarbonation starts as soon as the temperature drops. Already after a few days, most of the lost CO2 has been replaced with atmospheric CO2. The renewed carbonates are readily soluble in the acid hydrolysis process and their carbon and oxygen isotopes have a light signature. Fire-damaged historical mortars display the same features. If a long time has elapsed between hardening of the original mortar and the fire, the new carbonates have 14C concentrations that point to the fire event rather than to the building event. In several cases, the fire-damaged mortars have an easily soluble carbonate fraction with a 14C age that could be related to a major fire event, but still most of the soluble carbonate yields a 14C age that seems like a reasonable age for the original construction.
Chance discoveries of weapons, horse bones and human skeletal remains along the banks of the River Tollense led to a campaign of research which has identified them as the debris from a Bronze Age battle. The resources of war included horses, arrowheads and wooden clubs, and the dead had suffered blows indicating face-to-face combat. This surprisingly modern and decidedly vicious struggle took place over the swampy braided streams of the river in an area of settled, possibly coveted, territory. Washed along by the current, the bodies and weapons came to rest on a single alluvial surface.
The relative Bronze Age chronology for Scandinavia was established as early as 1885. It is traditionally divided into 6 periods (I–VI). Earlier attempts to make an absolute Bronze Age chronology for southern Scandinavia were derived from burials and settlements and were mainly based on radiocarbon-dated charcoal or carbonized cereals, often with undefined archaeological periods. Here, we present high-precision 14C dating on burials with well-defined associated archaeological periods in order to improve the absolute chronology of the Danish Bronze Age. Our results are in broad agreement with the traditional absolute chronology of the Danish Bronze Age. However, our results do indicate that the onset of period III likely occurred earlier than previously thought.
Within a project on Stone Age sites of NE Germany, 26 burials from the Ostorf cemetery and some further Neolithic sites have been analyzed by more than 40 accelerator mass spectrometry (AMS) dates. We here present the results of stable isotope and radiocarbon measurements together with reference 14C dates on grave goods from terrestrial animals such as tooth pendants found in 10 of the graves. Age differences between human individuals and their associated grave goods are used to calculate 14C reservoir effects. The resulting substantial reservoir effects have revealed misleadingly high 14C ages of their remains, which originally indicated a surprisingly early occurrence of graves and long-term use of this Neolithic burial site. We demonstrate that in order to 14C date the human bones from Ostorf cemetery, it is of utmost importance to distinguish between terrestrial- and freshwater-influenced diet. The latter may result in significantly higher than marine reservoir ages with apparent 14C ages up to ∼800 yr too old. The carbon and nitrogen isotopic composition may provide a basis for or an indicator of necessary corrections of dates on humans where no datable grave goods of terrestrial origin such as tooth pendants or tusks are available. Based on the associated age control animals, there is no evidence that the dated earliest burials occurred any earlier than 3300 BC, in contrast to the original first impression of the grave site (∼3800 BC).
Basal ice at the margin of the Greenland ice sheet was studied with respect to its physical characteristics and microbiological community. The basal ice contained high concentrations of dissolved ferrous Fe and must therefore be anoxic. Oxygen consumption experiments indicate that 50% of the oxidation was due to biological activity while the rest could be attributed to chemical processes, most likely weathering reactions with ferrous Fe. At least six different Fe-containing mineral sources were detected in basal ice together with potential bioavailable Fe nanoparticles. An active denitrifier population was identified due to formation of 30N-dinitrogen gas after amendment of anoxic sediment slurries with 15N-NO3−. Sulfate reduction could not be detected. The solid ice facies contained an abundant (∼108 cells cm−3) and complex microbial community that harbored representatives of at least eight major phyla within the domain Bacteria. The clone library was dominated by members of the β-subdivision of proteobacteria of which the largest proportion was affiliated to the genus Rhodoferax that comprises facultative aerobic iron reducers. The second most abundant phylum was Bacteroidetes. The solid ice facies had many physical similarities with the overlying debris-rich banded ice facies, indicating that they formed by similar subglacial processes and harbor similar microbial communities. This study extends our knowledge of life in subglacial environments such as beneath ice sheets. GenBank accession numbers: HM439882-HM439950; HQ144215-HQ144221.
Fifteen years of research on accelerator mass spectrometry (AMS) radiocarbon dating of non-hydraulic mortar has now led to the establishment of a chronology for the medieval stone churches of the Åland Islands (Finland), where no contemporary written records could shed light on the first building phases. In contrast to other material for dating, well-preserved mortar is abundantly available from every building stage.
We have gathered experience from AMS dating of 150 Åland mortar samples. Approximately half of them have age control from dendrochronology or from 14C analysis of wooden fragments in direct contact with the mortar. Of the samples with age control, 95% of the results agree with the age of the wood. The age control from dendrochronology, petrologic microscopy, chemical testing of the mortars, and mathematical modeling of their behavior during dissolution in acid have helped us to define criteria of reliability to interpret the 14C results when mortar dating is the only possibility to constrain the buildings in time. With these criteria, 80% of all samples reached conclusive results, and we have thus far been able to establish the chronology of 12 out of the 14 churches and chapels, while 2 still require complementary analyses.