Submitted by Rafael Santana (rafael.silvasantana@ufpe.br) on 2017-07-10T19:30:23Z No. of bitstreams: 2 license_rdf: 811 bytes, checksum: e39d27027a6cc9cb039ad269a5db8e34 (MD5) Dissertacao - Pedro Negrão.pdf: 2417925 bytes, checksum: 563fc37dbb3bf794487bc4e3c8fc102a (MD5) / Made available in DSpace on 2017-07-10T19:30:23Z (GMT). No. of bitstreams: 2 license_rdf: 811 bytes, checksum: e39d27027a6cc9cb039ad269a5db8e34 (MD5) Dissertacao - Pedro Negrão.pdf: 2417925 bytes, checksum: 563fc37dbb3bf794487bc4e3c8fc102a (MD5) Previous issue date: 2016-03-29 / CAPES / As argilas compõem um grupo de matérias-primas muito importante devido a suas múltiplas funções industriais. Em especial o caulim, possui propriedades físicas e químicas que possibilitam a sua utilização no processo industrial de uma grande gama de produtos, desde matéria-prima para a indústria cerâmica, de carga e cobertura de papel, entre outras. Esta pesquisa objetivou descrever, através da caracterização mineralógica, análise química, análise granulométrica, ensaios tecnológicos e de plasticidade, as características do material arenocaulinítico sondado no município de Igarassu – PE, ocorrência localizada próxima ao bairro de Nova Cruz 2. O material foi coletado através de sondagem a trado, tendo as amostras passado por análise mineralógica por difração de raios X, análise química por fluorescência de raios X, análise granulométrica, ensaios de plasticidade e foram confeccionados corpos de prova para a realização de ensaios tecnológicos. Os resultados obtidos foram comparados com as características de caulins de outros jazimentos descritos na literatura e com as especificações dos caulins aproveitados industrialmente. / Clays form a group of so important raw materials due to its multiple industrial functions. In particular, the kaolin has physical and chemical properties which allow its use at the industrial process a wide range of products from a raw material for ceramic industry, filler and paper coating, among others. This research aimed to describe through mineralogical characterization, chemical analysis, particle size analysis, technological tests and plasticity characteristics of sandy-kaolinitic materials collected in the city of Igarassu - PE, occurrence located near the Nova Cruz 2. The material was got by auger boring, the samples submitted to a mineralogical analysis through X ray diffraction, chemical analysis through X ray fluorescence, particle size analysis, plasticity tests and was prepared specimens to be performed for the technological tests. The results obtained were compared with the characteristics of kaolin of other deposits described in the literature and with the specifications of kaolin exploited industrially.

Fused glass beads as a sample preparation method for X-ray Fluorescence spectroscopy (XRF) were introduced in 1957 by Claisse; it soon became the preferred method to introduce oxide samples to the spectrometer, because heterogeneity, mineralogical and particle size effects are eliminated during the fusion process. Matrix effects are largely reduced by the resulting dilution. With the recent advances in XRF spectrometers, instruments with enhanced generator and temperature stability, improved sensitivity (even for light elements), and effective matrix correction software are available. Consequently, the largest proportion of analytical error results from the sample preparation step. Sampling error will always contribute the largest overall error but that is not the topic of this discussion. After more than 50 years of fused bead use in XRF analysis, certain matrices remain problematic. Although many fusion methods for chromite-, sulphide- and cassiterite-rich materials have been published, easily reproduced, routine methods for these still elude analytical chemists. Lengthy fusions at temperatures higher than 1100ºC are often prescribed for refractory materials and ores, and until recently one of the biggest challenges was a metal-bearing sample e.g. contained in slags or certain refractory materials. This study was conducted to identify and elucidate the reactions occurring in the formation of a lithium borate glass, but also between the lithium borate and oxides during glass formation. Different analytical techniques were used to investigate the reactions occurring during the fusion process based on theoretical glass-making principles. As a starting point, Thermo Gravimetric Analysis (TGA) and Differential Thermal Analysis (DTA) were used jointly to evaluate the reactions occurring during the fusion of lithium borate glasses, and at a later stage, oxide/flux mixtures. When a different TGA instrument was used, Differential Scanning Calorimetry (DSC) was used in conjunction with the TGA. Observed reactions were modelled in a muffle furnace to produce identical material in larger quantities, and this material was then investigated using X-ray Powder Diffractometry (XRD), Raman Spectroscopy and Electron Microprobe Analysis (EPMA). The most enlightening result from the TGA/DSC results was the large mass loss above 1050 ºC. Literature often prescribes prolonged fusions at elevated temperatures for certain fusions, but it was proved beyond reasonable doubt that this practise causes volatilisation of the flux and leads to erroneous analytical results. The next analytical technique applied to the flux and flux/oxide samples was XRD. Where pre-fused fluxes were investigated, the XRD data served as confirmation of the glassy state of the pre-fused flux as a broad humpy scan indicative of an amorphous material was seen in stead of a diffractogram with sharp, well defined peaks. After heating to above the temperature of re-crystallisation, the phases present could be identified from the diffractogram. Provisional results using the in-situ, high temperature stage point towards the possibility of using this technique to great effect to investigate the presence of different phases formed at high temperatures. Flux-oxide mixtures were measured on the high temperature stage and after cooling a new phase was observed indicating that new phases formed during a fusion reaction. As the heating stage is slow-cooled, the chance of crystallisation in the glass is good, providing the possibility for investigating this formation of new phases at elevated temperatures further with a more suitable heating element that will contain the material. Raman spectroscopy was subsequently used to gain information about the bonds within the flux. Pure lithium tetraborate and lithium metaborate fluxes were analysed as well as flux oxide mixtures. The vibrations could not be predicted from first principles as band broadening occurs in glasses that makes theoretical predictions very difficult. The data obtained was compared to similar studies in literature and good agreement was found. In oxide-flux mixtures definite new bands were observed that was not part of the flux or oxide spectrum. EPMA results allowed calculation of the maximum solubilities of an oxide in a specific flux. It was done using Cr2O3 and ZrO2 and compared well with experimental values obtained from literature. The microscope images revealed some new insights into the theory of XRF fusions. It could clearly be seen that dissociation of the minerals in the sample occurred, thus proving that no mineralogical effects exist in a fused glass bead, and it could be observed that the flux oxide mixture devitrify when over saturated. / Dissertation (MSc)--University of Pretoria, 2010. / Chemistry / unrestricted

SECO Tools manufactures tool inserts for all types of metal cutting machining. (Ti,W)C is a common raw material used in the production. At arrival, the material (Ti,W)C is always analyzed. Titanium has previously been analysed with x-ray fluorescence spectrometry, but as the calibration has previously been performed with two different types of titanium (rutile and metallic titanium), the results has differed. Because of that, this thesis project has been devoted to analyze titanium, to find the best titanium compound for producing standards. The work has been performed using literature studies and many experiments in the laboratories at SECO Tools inFagersta,Sweden. This project has included about ten working weeks. In this report the analysis methods of x-ray fluorescence spectrometry and spectrophotometry is described, as the methods has been used in the experiments. A big problem that was discovered during this project was the big standard deviation of results for the method used for analysing titanium with x-ray fluorescence. Because of that, much time of this project has been devoted to experiments trying to reduce the standard deviation between the samples, as this is vital to performing a reliable calibration. A variety of experiments has been performed without reducing the standard deviation between the samples to below 0.2 % -units for the (Ti, W) C-samples.

This dissertation consists of three articles that develop and implement geoarchaeological approaches to the study of hominin biogeography in the Greek islands, a region that may have played a key role during the initial peopling of southeastern Europe in the Middle to Late Pleistocene (770 – 13 ka). The first article addresses the need to find Palaeolithic sites in the Greek islands by reviewing geoarchaeologically informed archaeological surveys that prioritize deposits – Pleistocene sediments and soils – on mainland Greece. I operationalize and implement a four-phase approach for future deposit-centered surveys in the islands. I conclude that future surveys should target geomorphic settings conducive to paleosol preservation, such as in near-shore coastal areas (e.g., uplifted hillslopes and actively eroding alluvial fans) marked by paleo-sea-level-indicators (sea notches, marine terraces, and aeolianites), as well as sediment depo-centers (e.g., internally drained basins) in non-coastal geomorphic settings. The second article develops and employs a multiscalar geoarchaeological approach for investigating and interpreting complex hillslope formation processes at the newly excavated Palaeolithic site of Stelida, located on the island of Naxos, Greece. Here, I integrate traditional geoarchaeological methods (lithostratigraphy, pedostratigraphy, allostratigraphy) with microarchaeological techniques, such as thin-section soil micromorphology and portable x-ray fluorescence spectroscopy (pXRF) to separate sediments and soils aiding in the construction of a stratigraphic framework for Stelida.The third article further develops the method of integrating pXRF and soil micromorphology applied at the site-specific scale. In this article, I developed an Exploratory Spatial Data Analysis (ESDA) method for visualizing geochemistry-facies relationships through the application of pXRF to a resin-impregnated block sample preserving an Archaic (seventh century BCE) ash midden (eschara) from the site of Kalopodi, Greece.This dissertation addresses a primary research effort in Greece’s Aegean Basin (Greek islands): the search for and study of Palaeolithic archaeology dating to Middle and Late Pleistocene. Geoarchaeologically informed research designs, such as deposit-centered surveys in open-air environments, can increase Palaeolithic site inventories for the region by focusing on finding geomorphic settings conducive to paleosol preservation. Moreover, the multi-scalar geoarchaeological approaches here, which integrate sedimentology, pedology, micromorphology, and geochemistry, provide an effective approach for the identification and compositional (mineralogic and geochemical) study of paleosols within those settings.

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第21765号 / 工博第4582号 / 新制||工||1714(附属図書館) / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 河合 潤, 教授 神野 郁夫, 准教授 奥田 浩司 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

Analysis was performed on a 31-artifact sample of Late Terminal Formative obsidian excavated in 2003 from the archaeological site of Yugüe in the Lower Verde Valley of Oaxaca. This analysis was performed to determine the geochemical sources of the individual obsidian artifacts and replicate a prior study of Yugüe obsidian performed by David T. Williams for his thesis at the University of Colorado. This earlier analysis determined that five obsidian sources were present. Sourcing was accomplished using a handheld X-Ray fluorescence instrument and bivariate plotting of relevant trace elements. Five sources of obsidian were found during analysis: Pachuca, Otumba, Paredon, Guadalupe Victoria, and Zaragoza. Williams identified additional sources that were not identified in this study, but he also may have sampled artifacts from the site from other excavations. This previous analysis by Williams also did not attribute sources to individual artifacts, making it impossible for archaeological conclusions to be drawn about the life histories of particular artifacts. By attributing sources to individual artifacts during analysis, this project provides valuable context about both the site of Yugüe during the Terminal Formative period and the lower Rio Verde Valley.

Tropical latitudes play an important role in global climate as they export moisture and energy pole-ward. Recent tests of predictive climate models against Holocene paleoclimate data show discrepancies between predicted and observed values in Tropical regions. Terrestrial paleoclimate records could help resolve these discrepancies by all allowing for better understand of the sensitive ocean-atmosphere climate dynamics in the tropics and by providing additional information from a diverse source of proxies. The Caribbean is an ideal location for study as its climate is influenced by both the Atlantic and Pacific Oceans. However, there are relatively few sources of paleoclimate proxies in this region due to its archipelagic nature. If Caribbean climate is to be thoroughly investigated, additional environments and climate proxies need to be investigated. As coastal systems are ubiquitous throughout the Caribbean, they are ideal for investigation of Holocene paleoclimate in this region. However, they can be ephemeral on millennial timescales making them challenging to use in paleoclimate analysis. This dissertation discusses new methods and basins that facilitate the study of these systems. Several important contributions have been made by this thesis. (1) Core scanning XRF data, when examined with additional proxies such as foraminifera, can be used to infer shifts in regional precipitation patterns in a coastal setting. Though these methods have been used before in deep basins, this represents the first use of core scanning XRF in a littoral setting. (2) The evolution of sinkhole sedimentation is reliant on both the morphology of the sinkhole and water level within the feature. This thesis shows that coastal systems are a viable source of paleoclimate information and which can hold valuable information for reconstructing climate. / Thesis / Master of Science (MSc)

<p>Alzheimer’s disease (AD) is a progressive neurodegenerative disease affecting more than 6 million individuals in the United States and more than 50 million worldwide. Currently, there exists no cure for AD and there are very few treatments to limit disease progression. Understanding the mechanisms through which AD develops and the risk factors associated with disease onset and progression is imperative in diagnosis and treatment of AD. Metal dysregulation has been implicated in disease pathogenesis through a number of mechanisms. Toxic heavy metals, such as lead (Pb) and mercury (Hg) are known to have deleterious effects on the central nervous system (CNS) and have been shown to increase AD pathology in animal models. However, there are significant knowledge gaps on how these metals deposit in human and animal brains at the microscopic scale, how they interact with essential metals in brain, and the relation of heavy metal exposure and AD. In this project, we aimed to investigate the distribution of heavy metals and their interactions with essential elements in transgenic mouse and human brain tissue models. We report, for the first time, Pb distribution and its co-deposition with Se in mouse brains following subchronic Pb exposure, Hg distribution and its co-deposition with Se in post-mortem AD and no cognitive impairment (NCI) brains, and the association of Pb, Hg, and other metals in these brains. All the data were obtained using synchrotron x-ray fluorescence (XRF), a powerful technique that allows for localization and quantification of multiple biological elements, as well as heavy metals, with a high spatial resolution and low detection limit. The work will shed light on the role essential metals, especially Se, play in neurotoxicity of Pb and Hg, and pave the way for potential future directions on heavy metal exposure and neurodegeneration.</p>

This study assessed ways compositional analysis, facilitated by portable X-ray fluorescence technology (PXRF), can be applied in the museum setting to resolve provenance issues and other collections management questions. A major segment of the study evaluated PXRF as a non-invasive geochemical analysis technique to address concerns about whether the resolution of results is sufficient to draw meaningful conclusions. Compositional analysis, mainly facilitated by PXRF, was successfully applied to three clay artifact collections from the southwestern United States. Pottery sherds from Fourmile Ruin were analyzed using PXRF and compared to analyses from invasive wavelength-dispersive XRF and X-ray diffraction techniques. Expanding the data associated with the artifacts increases the collection's research value. The results of hierarchical clustering suggest further compositional analysis of Fourmile Ruin ceramics to verify this study's conclusions and evaluate current assumptions regarding where certain wares are produced. The iconic Pilling figurine collection was analyzed using scanning electron microscopy and PXRF to evaluate the authenticity of a figurine that had been returned after being lost for forty years. The geochemical tests confirmed the results from the basketry-imprint analysis that the returned figurine was the missing figurine, allowing the museum to restore the artifact's provenance. A pot being offered as a potential donation was analyzed using PXRF to evaluate if there was evidence of forgery or previous repair and help the museum decide whether or not to accept the donation. The study concluded the vessel has not been constructed or partially reconstructed using plaster of Paris. If the vessel has been constructed or partially reconstructed using pieced-together pottery sherds, they all came from a similar clay source. Based on these results, the museum decided to accept the pot as a donation. This study demonstrates the viability of PXRF as a useful geochemical research technique, particularly in cases where higher resolution invasive and destructive analysis techniques are not permitted. It establishes that PXRF can be used to authenticate and restore provenance both within a collection of objects and within a single object. Compositional analysis facilitated by PXRF can be a valuable tool in museum collections management and research.

No description available.