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Prehistoric shell mounds can be useful for the quantification of the radiocarbon marine reservoir effect (MRE) and, at the same time, knowledge about the MRE allows for the establishment of robust chronologies for these sites. This creates a loop in which the archaeological setting has a dual role: it is part of both the method and the application. Therefore, it is paramount to address these sites from both archaeological and environmental perspectives, investigating their origin and diagenesis in order to overcome biases caused by post-depositional alterations. In this study, samples of bone, charcoal and shell from a Late Holocene shell mound in Southern Brazil, the Sambaqui de Cabeçuda, were analyzed following a multidisciplinary approach to disentangle the complex relationships between archaeology and the environment. We performed X-ray diffraction, radiocarbon dating, stable isotopes (δ13C, δ18O, δ15N) and anthracology analyses as well as Bayesian Chronological Models and Isotope Mixing Models to assess the local MRE and to reconstruct the diet of Cabeçuda builders. Our results reveal a negative local correction for the MRE (ΔR = –263 ± 46 14C yr), expected for the lagoon next to the site, and diets with considerable intakes of marine proteins. We examine the implications of these results for the chronology of the site and discuss a series of complications when performing MRE studies using shell mound sites.
Isotopic analysis of Micropogonias furnieri otoliths were used to get insight into palaeoceanographic conditions in the Guanabara Bay and Saquarema Lagoon, Rio de Janeiro state (RJ), located on the southeastern coast of Brazil, under upwelling influence of the Cabo Frio system. Archaeological otoliths come from two Holocene shellmounds (or sambaquis): Galeão and Beirada. For the first time, radiocarbon analysis using high accuracy techniques were performed at Galeão. Age range was determined to be between 5820 and 4980 cal BP, which extends the chronology of human settlement in the Guanabara Bay. Micro-samples of the otoliths were collected sequentially from the core to the edge, to provide continuous δ18O and δ13C isotopic profiles over the lifetime of the individual fish. Derived-δ18Ooto palaeotemperature estimates vary according to seasonality, resulting in a palaeoceanographic variation between 8 to 31°C for Guanabara Bay and 8 and 28°C for the Saquarema Lagoon. Our data indicate that whitemouth croakers were captured during the Middle Holocene from the Guanabara Bay and Saguarema Lagoon and resided in cooler temperatures compared to temperatures of current conditions.
Many organisms living in the ocean create tests, shells, or related physical structures of calcium carbonate (CaCO3). As this is most often from dissolved inorganic carbon, using organisms that create calcium carbonate structures for climate research and dating purposes requires knowledge of the origin of carbon that is incorporated. Here, we give a short overview of research on marine carbonates over the last 60 years, especially that based on shell and coral samples. Both shells and corals exhibit annual growth patterns, like trees, and therefore offer possibilities for yearly resolution of past radiocarbon (14C) variations. We concentrate on their evolution in 14C dating including difficulties in determining reservoir ages as well as the possibilities they offer for archaeological dating, oceanography, calibration purposes as well as environmental research in general.
The vermetidae fossils of Petaloconchus varians, formed by calcium carbonate, associated with their radiocarbon ages, are the most accurate indicators of paleo sea level due to their restricted occupation in the intertidal zone in the rocky shore. However, the recrystallization of minerals can affect these age calculations and, consequently, the interpretation of the data. The aim of this study is to present new indicators of paleo sea-level changes in Southeast Brazil for the last 6000 years contributing to fill the data gap for the late Holocene. The influence of the recrystallization process was successfully resolved using the CarDS protocol, enabling the separation of the original aragonite fraction by density, prior to radiocarbon dating. This avoids the rejuvenation of ages and ensures greater efficiency for data interpretation. Paleo sea-level indicators were able to show a progressive increase in sea level up to the transgressive maximum of 4.15 m in 3700 BP years, followed by a regression to the current zero. This regression seems to have in addition, here we reinforce the reliability of the use of fossil vermetids as indicators of sea-level fluctuations.
Fossil fuels are of utmost importance to the world we live in today. However, their use can cause major impacts on the environment, especially on water resources. In this regard, algae have been intensively used as a strategy for remediation and monitoring of environmental pollution due to its efficient absorption of contaminants. In this work, samples of seaweed collected in Niterói/RJ—contaminated with kerosene and diesel—were analyzed by radiocarbon (14C) accelerator mass spectrometry (AMS) and by n-alkane quantification with gas chromatography to evaluate bioaccumulation in function of the dosage of contaminants. The biogenic content measured by radiocarbon analysis resulted in 95.6% for algae contaminated with 10 mL of kerosene and 67.6% for algae contaminated with 10 mL of diesel. The maximum intensity of n-C17 n-alkane in algae with 5 mL, 10 mL, and 15 mL of diesel was 768.2, 1878.1, and 5699.2 ng.g-1, respectively. While the maximum concentration of n-C27 in algae with 5 mL, 10 mL and 15 mL of kerosene was 3.3, 35.9, and 150.3 ng.g-1. We concluded that, for both contaminants, their incorporation into algae increases as the contamination dosage increases, making this methodology an effective technique for monitoring and remediation of urban aquatic ecosystems.
Since the establishment of the first radiocarbon accelerator mass spectrometry facility in Latin America in 2009, the Radiocarbon Laboratory team of Universidade Federal Fluminense (LAC-UFF) has worked to improve sample preparation protocols and increase the range of environmental matrices to be analyzed. We now present the preliminary results for DIC sample preparation protocols. The first validation tests include background evaluation with pMC value (0.35 ± 0.04) using bicarbonate dissolved in water. We also analyzed surface seawater resulting in pMC value (101.38 ± 0.38) and a groundwater previously dated from LEMA AMS-Laboratory with pMC value (12.30 ± 0.15).
In paleoenvironmental research, several proxies are used to reconstruct climate and vegetation. The establishment of a chronological framework allows for the association of different proxies and correlation of events happening in different geographic areas. Cultural deposits, such as the shellmounds found along the coast of Brazil, play an important role in paleoenvironmental interpretations. Here, we have employed anthracological analysis in charcoal fragments from the Amourins shellmound, located at the margins of the Guanabara Bay, Rio de Janeiro. This allowed for the taxonomic identification and selection of short-lived trees and specific parts of plants for accurate radiocarbon dating. We recorded genera and families typical of the Atlantic Forest, restinga forest, open restinga and mangrove. The 14C ages of charred nuts from different occupational layers range from 3807 ± 35 to 3503 ± 70 BP and a sequential chronological model was built, relating the predominance of mangrove vegetation to the period between 4130–3960 cal BP.
The Radiocarbon Laboratory of the Fluminense Federal University was installed in 2009, and its NEC Single Stage Accelerator Mass Spectrometry system has been operational since 2012. As the first 14C-AMS facility in Latin America, the LAC-UFF became a reference center for radiocarbon (14C) dating in Brazil. Over the years we have implemented pretreatment protocols for several kinds of materials, such as cellulose, soil, bone, and biofuels. In the present paper we describe our current protocols for the preparation of these types of samples. Moreover, after 10 years of operation, with the aim of expanding the range of materials we are able to analyze, we report the results of several tests to improve accuracy, precision and background levels. For example, here we discuss how isotopic fractionation during the graphitization and measurement steps has been controlled. Concerning results interpretation, our research group has been using OxCal chronological models to analyze different contexts such as stromatolite growth, tree rings, soil deposition and marine reservoir effect (MRE) determination.
Collagen extraction depends on the state of bone preservation, and the acidity of Brazilian soils often prevents the use of this material for radiocarbon dating. When available, however, bone samples constitute very important chronological records for both archaeological sites and natural depositional sites of specific animals. The extraction of collagen was performed using two filters, the first aiming to remove insoluble contaminants, and the second, a vivaspin ultrafilter 30KD to retain large molecular weight materials. The collagen was liofilized and converted to CO2 by combustion in sealed quartz tubes with CuO and Ag. The graphite was produced by zinc reduction in independently sealed Pyrex™ tubes. In order to verify the accuracy of this protocol, we analyzed a modern bone and four previously dated fragments, including those from the Sixth International Radiocarbon Intercomparison (SIRI), and a fragment of human bone from the Amourins site, a Brazilian shellmound. The results for the known age material are in agreement with the expected and the studied sector of Amourins shellmound was dated 4100–3900 years cal BP from a chronological model performed with charcoal dating found in different stratigraphic layers. Samples were dated at the radiocarbon laboratory of Universidade Federal Fluminense (LAC-UFF) in Brazil.
In a wave-dominated coast, most of the Jacarepaguá coastal plain is occupied by buildings. During a new construction in this region at Barra da Tijuca, the subsurface area was excavated, exposing its quartzose sand nature, with a high mollusk shell concentration and in situ echinoderms at –10 m depth. The possibility to access this area encouraged us to investigate the evolution of the coastal plain. A 7.84-m-long core was recovered by percussion drilling. Stratigraphic, grain size, and geochemical analysis were undertaken. Three carbonate samples were dated by radiocarbon accelerator mass spectrometry (14C AMS). The revised sea-level variation curve revealed that the last postglacial marine transgression reached the present mean sea-level at 7945–7500 cal BP. The sandy deposit bottom was an ancient shoreface, with in situ echinoderms buried at 7770–7540 cal BP by the Pleistocene inner barrier reworking due to the last marine transgression. The Holocene outer barrier-lagoon and its flood tidal delta were formed from 5440–5070 cal BP. Mid-Holocene marine regression allowed the outer barrier progradation and the lagoon shallowing/infill. This paper confirms prior models proposed by other researchers for the Rio de Janeiro central coast and shows its similarity with the New South Wales coast, Australia.
Identifying and tackling recrystallization is a critical factor in the reliable radiocarbon (14C) dating of carbonates, since exogenous carbon can be incorporated and thus mask the real age of the samples. Vermetids are among the most important bioindicators used for paleo sea-level reconstruction, and the accuracy of their chronology can significantly impact sea-level curves. Age differences larger than 1 14C kyr before and after acid etching, combined with X-ray diffraction (XRD) analysis that indicates a significant amount of calcite still remains in the shell, led us to apply the previously developed carbonate density separation protocol (CarDS). Using a solution of sodium polytungstate, with density of 2.80 g/cm3, we successfully separated different carbonate fractions for a set of 10 vermetid samples from the coast of Rio de Janeiro, southeast of Brazil. Each separation was verified by XRD analysis and the 14C concentrations of different fractions were compared. The results show that the calcite fraction in the studied vermetid samples varied from 12 to 63% and aragonite fraction ages are up to 2 14C kyr older than the raw samples, thus confirming the efficacy of CarDS in removing young carbonates and the importance of density separation to vermetids prior to accelerator mass spectrometry (AMS) dating.
The Rio Grande Cone is a major fanlike depositional feature in the continental slope of the Pelotas Basin, Southern Brazil. Two representative sediment cores collected in the Cone area were retrieved using a piston core device. In this work, the organic matter (OM) in the sediments was characterized for a continental vs. marine origin using chemical proxies to help constrain the origin of gas in hydrates. The main contribution of OM was from marine organic carbon based on the stable carbon isotope (δ13C-org) and total organic carbon/total nitrogen ratio (TOC:TN) analyses. In addition, the 14C data showed important information about the origin of the OM and we suggest some factors that could modify the original organic matter and therefore mask the “real” 14C ages: (1) biological activity that could modify the carbon isotopic composition of bulk terrestrial organic matter values, (2) the existence of younger sediments from mass wasting deposits unconformably overlying older sediments, and (3) the deep-sediment-sourced methane contribution due to the input of “old” (>50 ka) organic compounds from migrating fluids.
Given the difficulty in obtaining robust chronologies from tree rings in tropical regions, the search for appropriate species is very important. Both dendrochronology and radiocarbon (14C) measurements are required to validate the use of any specific tree. Some species have proved to be reliable for representing atmospheric 14C concentration over time, such as Cedrela fissilis and Araucaria angustifolia. However, not only the species have to be validated, but also different climatic conditions may result in different growth patterns for the same species. In this work, we study the annual growth rings of Cedrela fissilis from a dry tropical forest patch typical of a highly seasonal climate in central Brazil. 14C accelerator mass spectrometry (AMS) was used to compare the isotopic ratios of tree rings with the 14C concentrations in the atmosphere during the nuclear tests based on curve Bomb13SH 1-2. Results are similar to the bomb peak curve within the period from 1958 to 1980 AD and serve as a crucial test for the cross-dating analyses using the skeleton plot technique.
The Abrolhos bank, in southern Bahia State (BA), is the largest coral reef system in the southwestern Atlantic. It is highly influenced by the Brazil Current (BC), since it is located in the continental shelf. By contrast, Todos os Santos Bay (TSB), in Salvador, capital of Bahia State (BA) has an important coral biodiversity, located in a bay inlet with restricted water circulation. Coral cores were collected in those sites and were analyzed for density band counting and by Th/U dating to estimate growth rates and age. In this work, we present 14C ages of some of these bands in order to evaluate the marine reservoir effect (MRE) to which the colonies were subjected during growth. It is the first study making use of coral skeleton samples for MRE determination for the Brazilian coast. ΔR was calculated to be –151±23 14C yr, while that for the TSB was –107±51 14C yr.
The radiocarbon (14C) chronology of hunter-fisher-gatherers’ archaeological settlements along the Brazilian coast is usually based on mollusk shells, charcoal from hearths, and eventually human bones. However, fish otoliths are found in several archaeological contexts and may represent a reliable option as a chronological record. In this work, we compare the 14C dates of whitemouth croakers (Micropogonias furnieri) otoliths with dates obtained from other materials (shell and charcoal), collected from shellmounds on the coast of Rio de Janeiro, with the aim of improving the accuracy in the 14C dating of Brazilian shellmounds, strengthening the comprehension of the native populations’ occupational trends and the coeval palaeoceanographic context. Based on x-ray diffraction results for archaeological otoliths, their geochemical composition indicates minimal diagenesis effect over time even under burial conditions in the studied sites. The comparison between otolith dates and dates obtained from other proxies revealed similar results but with decreased deviations in otolith dates in all of the studied sites.
Considering the impact of coastal dynamics on the radiocarbon (14C) marine reservoir effect (MRE), upwelling has the potential of enhancing marine influence, usually 14C depleted. Freshwater input can contribute either to increased reservoir offsets, when dead carbon from rock weathering is available, but also towards an atmospheric 14C signal, when the presence of terrestrial organic matter from catchment prevails. An overview of the MRE studies based on shellmounds on the coast of Rio de Janeiro reveals a pattern of negative local corrections for Saquarema and Rio das Ostras but positive values for Cabo Frio island, suggesting the presence of cold upwelling waters in Cabo Frio at 1.6–1.2 cal kBP. New results for a shellmound on the Ilha Grande island, in the western portion of the Rio de Janeiro coast, revealed a negative value at about 3 ka. We discuss distribution of MRE values and temporal variability in the region and their relation to ocean dynamics, continental input and the choice of marine organisms used for ∆R determination. A comparison of local reservoir offsets for the Saquarema region obtained from fish otolith and mollusk shells revealed similar ΔR distributions, showing that both materials can be equally used.
Among the oldest remains of living beings to have inhabited the Earth’s surface, there are the stromatolites—laminated sedimentary rocks associated with lithified mats of layered phototrophic microbial communities—which grow in specific environmental conditions. In the present work, we study a recent carbonatic stromatolite from Lagoa Vermelha (Rio de Janeiro, Brazil), a shallow coastal hypersaline lagoon. X-ray diffraction was associated to a depth chronological model defining three different sections based on changes in mineral composition of the stromatolite with increased dolomite content. Although a mean growth rate of 0.19±0.03 mm/yr is observed, the model discloses decreasing growth rates among the sections. Since dolomite formation can be related to high availability of Mg+2, confirmed by an expressive presence of (Ca, Mg)CO3, the lower growth rates were associated to a more arid environment, until approximately 1440 cal AD, with higher temperatures and consequently promoting water evaporation and salinity enhancement.
Jaguariaíva 1 is a sandstone rockshelter located in Jaguariaíva, Paraná State, Brazil, with rock art on the surface of the walls and ceiling. A stratigraphic analysis of the soil within the shelter showed six occupational layers and a superficial disturbed layer with evidence from the end of the 19th century. The establishment of a rock-art chronology became possible using fallen painted rock sections incorporated into three sedimentary levels underlying this rock shelter. These show superimpositions of several pictures of differently sized animals, such as deer, and lattice motifs, which are generally associated with the Planalto rock art tradition. The chronological study was performed based on radiocarbon (14C) analysis of charcoal collected from six excavated subsurface archaeological contexts. The two oldest layers, associated with hunters and gatherers of the Umbu tradition, were dated to 7680–7516 cal BP and 6913–6656 cal BP. There are four occupational layers from ceramists and farmers related to the south Jê linguistic family, and linked to the Itararé-Taquara archaeological tradition: layer 3 linked to the oldest of such occupation, dated to 3058–2796 cal BP, followed by layer 4, dated to 2080–1701 cal BP. Layers 5 and 6, dated to 1995–1526 cal BP and 540–152 cal BP, respectively.
Among other zooarchaeological remains, terrestrial snails’ shells from the Thaumastus and Megalobulimus genera are found in some Brazilian shellmounds, presenting a potential substitute for charcoal in radiocarbon dating analyses, as reliable representatives of the atmospheric carbon isotopic ratio. In this paper, we present statistically similar results of both charcoal and land snails samples from the same archaeological contexts in three settlements on the coast of Rio de Janeiro. The Manitiba I shellmound results range from 4.2 to 3.7 ka cal BP (95.4%), contemporary with the Saquarema shellmound, occupied during the period from 4.3 to 3.6 ka cal BP (95.4%). For the Usiminas shellmound, two groups of samples revealed different periods of time for two occupational layers from 2.3 to 2.1 ka cal BP (95.4%) and from 1.6 and 1.3 ka cal BP (95.4%). A model constraining each group of samples to within a single phase has a general agreement of 97% with only two outliers out of 22 dates, yielding minimum individual agreement of 74% and 7% posterior outlier probability for Saquarema shells. These are good examples of sites in which the occupation chronology can be successfully obtained by the radiocarbon dating of land snails.