Unconventional gas reservoirs in carbon dioxide sequestration activities is a relatively new and unexplored concept currently undergoing pilot scale testing. Sequestration has the potential for enhancing gas recovery while mitigating carbon dioxide to long term storage structures. Due to the extremely complex systems associated with these unconventional reservoirs, modeling becomes difficult to predict accurately. This thesis presents methods to increase the confidence of inferred parameter testing for unconventional reservoir sequestration in both seam coal bed methane wells and a shale wells. Various tests include the use of computed tomography coupled with Avizo modeling software, inductively coupled mass spectrometer fluid transport analysis, pressure transient build tests, liquid level detection, and desorption analysis coupled with cleat image analysis. Analyses of coals performed by both environmental scanning electron microscope (ESEM) and micro CT demonstrate that distributions of cleat porosity in coals are anisotropic and not correlated to the seam depth or location. ESEM is used with micro CT scanning to verify the results before and after the impregnation of the carbonic acid. The micro CT data in Avizo Fire© was used calculate an increase in cleat permeability by 25%. The increase of major flow pathways is caused by the dissolution of carbonates. Changes in the structures were observed qualitatively through ESEM and micro CT and quantitatively through Avizo and inductively coupled mass spectrometry. The results of comparative study between the cleat structures and the desorption of various seams indicate a trend in the cleat porosity and the desorption rate of the coals as well as the cleat porosity and the total gas in various seams. / Master of Science

This work deals with the evaluating of the signal level value from the sample in the environmental SEM. In work there were processed the comparison of the osciloscopic method for the evaluating of the signal level value in the environmental SEM, the method for the evaluating of the signal level from the grey level of the sample images and the method for the evaluating of the signal level from the osciloscop. There are described the advantages and disadvantages of the methods and procedures for processing the methods.

The thesis deals with the scintillation secondary electron detector for environmental scanning electron microscope, its design and construction. The starting point was numerical simulation of electrostatic fields and electron trajectories in the electrode system of the detector and simulation of pressure distribution and flow of gases in different parts of the detector. On the basis of modeling and simulation, construction changes of the detector were gradually implemented. Detection efficiency of each version of the detector was determined by the method described in the work. This method enables to evaluate signal level from the captured images of the specimen, quality of images was stated from signal to noise ratio. The thesis describes the whole process of the detector improvement from initial state, when the detector operated with lower efficiency in the pressure range from 300 to 900 Pa, to final version that enables usage of the detector in the range from vacuum up to 1000 Pa of water vapors in the specimen chamber of the microscope.

A ação do instrumento endodôntico nas paredes do canal leva à formação de debris dentinários. Sua remoção é principalmente função das manobras de irrigação. Entretanto, a ação do instrumento pode facilitar ou não o acúmulo dos debris dentinários, principalmente em função da sua cinemática. O sistema Twisted File (TF) Adaptive (SybronEndo, Orange, CA) combina o movimento rotatório contínuo e reciprocante e o sistema Reciproc (VDW, Munique, Alemanha) realiza o preparo do canal radicular pelo movimento reciprocante puro. Os objetivos deste estudo foram, utilizando a microtomografia computadorizada (micro-CT): avaliar, ex vivo, o preparo (aumento de volume e superficies não preparadas) e quantificar o acúmulo de debris dentinários em canais ovais longos comparando os sistemas TF Adaptive e Reciproc; avaliar o efeito da irrigação ultrassônica ativada intermitente (IUAT) após o preparo químico-cirúrgico com os sistemas propostos, na redução de debris dentinários; e relacionar a presença de debris dentinários com o magma dentinário avaliado por meio do microscópio eletrônico de varredura. Canais distais de trinta e oito molares inferiores foram selecionados e divididos em dois grupos: G1 - TFA (n=19) e G2 - RC (n=19). Cada espécime foi submetido a três escaneamentos: prée pós-operatório e pós-irrigação ultrassônica passiva final. Após a reconstrução das imagens resultantes dos três escaneamentos, foi feito o corregistro das mesmas com o programa DataViewer. Os programas CTAn e CTvol foram utilizados para binarização dos objetos de interesse, avaliações morfométricas e reconstrução dos modelos tridimensionais. Foram mensurados o aumento de volume do canal, as superfícies não preparadas e os debris dentinários após o preparo químico-cirúrgico. Após a irrigação final, cinco raízes de cada grupo foram clivadas longitudinalmente ao meio no terço apical e analisadas no microscópio eletrônico de varredura (MEV) quanto à presença de magma dentinário. O sistema de pontuação utilizado foi o de Hülsmann et al. (1997). Os resultados foram analisados pelo programa Bioestat e mostraram uma distribuição não-paramétrica pelo teste D\'Agostino. Por esta razão, para a análise dois a dois entre os grupos foi utilizado o teste de Mann-Whitney. Na análise intra-grupo, o teste de Kruskal-Wallis foi o escolhido, com complementação do teste de Dunn quando necessário. Os dados obtidos mostraram que o sistema TF Adaptive removeu mais dentina quando todo canal foi considerado (p<0,05). Entretanto, não houve diferença estatisticamente significante quanto à porcentagem de superfície não preparada em ambos os sistemas (p>0.05). Em relação ao acúmulo de debris dentinários e redução de debris dentinários pós-irrigação ultrassônica passiva, também não houve diferença entre os grupos (p>0.05). A IUAI promoveu redução significativa de debris dentinários, à exceção do terço apical. Qualitativamente, no MEV, observou-se magma dentinário não-homogêneo cobrindo a parede do canal, especialmente no grupo Reciproc. Conclui-se que nenhum sistema conseguiu preparar completamente as paredes de canal radicular oval longo e que a IUAI reduz os debris dentinários na ordem de 60-70%. Na análise do MEV, pode-se observar que não houve correlação entre a redução de debris dentinários e o magma dentinário. / The action of the endodontic instrument leads to hard-tissue debris. The main goal of the irrigation procedures is its removal. Nevertheless, depending on its kinematics the rotary file can contribute to the removal of hard-tissue debris. The TF Adaptive system (SybronEndo, Orange, CA) combines the rotary and reciprocating movement and the Reciproc system (VDW< Munique, Alemanha) with pure reciprocating movement, removes significant quantities of dentin of the canal wall with more difficulties of pulling out hard-tissue debris. The aims of this study were, using microcomputed tomography: evaluate preparation and quantify hard-tissue debris reduction in long-oval canals comparing TF Adaptive and Reciproc systems; evaluate the effect of passive ultrassonic irrigation (PUI) after preparation with the proposed groups in the accumulation of hard-tissue debris; and correlate the presence of hardtissue debris with smear layer evaluated by scanning eléctron microscope (SEM). Distal canals of thirty-eight lower molars were selected and divided in two groups: G1 - TFA (n=19) and G2 - RC (n=19). Each specimen was scanned three times: preand post-instrumentation of the root canal; and post-passive ultrassonic irrigation. After reconstruction of the scanned images, a co-registration was done with DataViewer. The softwares CTan and CTvol were used for binarization of the objects of interest, morphometrics alterations and reconstruction of tridimensional models and hard-tissue debris models. Volume increasing, non-prepared surfaces and hardtissue debris after instrumentation were measured. After final irrigation, the root canals were clived in halves at the apical third and analyzed by scanning eléctron microscope related to smear layer. The score system described by Hülsmann et al. (1997) was used. The results showed a non-parametric distribution by D\'Agostino test. For that reason, Mann-Whitney test was used to compare the experimental groups and the Kruskall-Wallis test to compare intra-group performance. Dunn test determined which sample was different. Data shows that TF Adaptive removed more dentin in the whole root canal (p<0,05). There was no significant statistic difference comparing non-prepared surfaces between the systems (p>0,05). Related to hardtissue debris and reduction of hard-tissue debris after passive ultrassonic irrigation, there was no significant difference between TF Adaptive and Reciproc. The PUI reduced significantly hard-tissue debris, except for the apical third. The scanning electron microscope (SEM) showed a non-homogeneous smear layer covering the canal dentin walls, specially the Reciproc group. It was concluded that no system completely prepared the dentin walls of long-oval root canals and the passive ultrassonic irrigation decreased hard-tissue debris about 60-70% in the evaluated systems. SEM analysis reported no correlation between hard-tissue reduction and smear layer.

Esta pesquisa apresenta os resultados obtidos com o emprego de um método físico para aumento da resistência de concretos projetados a pequenas idades. O método consiste na aplicação de gradientes elétricos ao material logo após a projeção, sendo mantido nas primeiras 5:30 h de hidratação. O comportamento mecânico do concreto projetado submetido a gradientes elétricos foi analisado em termos da resistência à compressão e módulo de elasticidade a partir da resposta de modelos estruturais e de amostras extraídas de estruturas projetadas em diferentes idades. Os modelos estruturais foram desenvolvidos para simular esforços ao concreto projetado semelhantes àqueles resultantes da interação solo-suporte em obras subterrâneas. A projeção do concreto nestes modelos ocorreu diretamente sobre o solo, permitindo assim a análise da eficiência do método sob condições de fuga de corrente elétrica para o maciço em diferentes tipos de solos. A instrumentação destes modelos permitiu analisar a eficiência do método sobre a deformabilidade do concreto projetado, sendo medidas as evoluções de deformações elásticas e deformações de fluência ao longo do tempo bem como deformações independentes de tensões desde as primeiras horas de hidratação. Constataram-se acréscimos na resistência nas primeiras 8 h de idade do concreto projetado em projeção sobre placas de madeira e diretamente sobre o solo. O módulo de elasticidade obtido a partir da instrumentação da resposta instantânea ao carregamento também constatou melhorias pela aplicação do gradiente elétrico. A reologia do concreto projetado, a partir das parcelas de deformações instantânea, retardada e lenta foi analisada utilizando-se o modelo proposto por SCHUBERT (1988). Melhorias foram observadas na resposta em termos de deformações do concreto projetado quando submetidos ao gradiente elétrico, apresentando menores taxas de evolução de deformações lentas em resposta a carregamentos iniciados em idades inferiores a 10 h e redução da parcela de deformação permanente frente ao descarregamento. A investigação dos fatores que provocam acréscimos na resistência a pequenas idades pela aplicação de gradientes elétricos a pastas e argamassas foi realizada utilizando-se técnicas de Microscopia Eletrônica de Varredura e Difratometria de Raio X. Constataram-se alterações na microestrutura de argamassas submetidas a gradiente elétrico, sem alteração nos compostos hidratados. Alterações na taxa de hidratação foram evidenciadas pela comparação de padrões difratométricos entre pastas submetidas a gradientes elétricos e pastas de referência. / This work presents the results obtained by employing a physical method for the strength increase of shotcrete at early age. The method consists of applying electric gradient to the material during the first 5 hours and 30 minutes of hydration, starting immediately after spraying. The mechanical behavior of shotcrete subjected to electric gradient was evaluated at different ages in terms of unconfined compressive strength and elastic modulus obtained from the response of structural models and on samples cored from the structural models. Shotcrete structural models were constructed in order to simulate internal forces resulting from ground mass - support interaction in underground works. Shotcrete in these models was sprayed directly on soil. It was thus possible to analyse the efficiency of the method when leakage currents occur through the soil. Model instrumentation alloed to evaluate the method efficiency in terms of shotcrete deformability. The evolution of elastic and creep strains were evaluated, as well as stress-independent strains since the beginning of hydration. Strength increase during the first 8 hours of age were observed both on panels shotcreted on wooden forms and directly on soil. The elastic modulus was also obtained from the analysis of the instantaneous strain reponse to the applied load. Improvement due to electric gradient was also found this way. Shotcrete rheology in terms instantaneous, delayed and creep strains was analyzed adopting the model proposed by SCHUBERT (1988). Improvement due to the electric gradient was found with respect to each of those strain components resulting from load applied at ages lower that 10h. Permanent strain after unloading was also reduced. The investigation of the phenomena responsible for the strength increase at early age due to the application of electric gradient to cement paste and mortar was carried out with the techniques of scanning electron microscope and X-ray diffraction. Microstructure changes were found in mortar speciments subjected to electric gradient, however without any change of hydrated products. Hydration rate changes were detected from diffractometric patterns of cement pastes subjected to electric gradient.

O presente estudo in vitro analisou o efeito de 3 sucos de fruta com baixo pH (suco de cupuaçu, taperebá e laranja), e saliva artificial (controle) sobre materiais restauradores indicados em lesões cervicais não cariosas: resina composta nanoparticulada (Filtek Z350 XT), cimento de ionômero de vidro resino modificado (Vitremer) e um cimento de ionômero de vidro convencional (Fuji II). Os materiais foram avaliados, quantitativamente, quanto à alteração de: peso, rugosidade superficial e microdureza superficial, e qualitativamente, por microscopia eletrônica de varredura (MEV). Foram confeccionados 144 corpos de prova para cada teste quantitativo (n=12) e 45 para o MEV (n=3), de (8mm de diâmetro x 2mm de altura). Os corpos de prova foram preparados, mantidos em saliva artificial por 24 h à 37º C, receberam acabamento em politriz, e em seguida foram realizadas as leituras iniciais. Durante um período de 10 dias consecutivos, os corpos de prova foram submetidos ao desafio erosivo (nos respectivos sucos de frutas) durante 30 minutos três vezes ao dia, totalizando 90 minutos/dia e mantidos em saliva artificial entre os intervalos. Após o período de ciclagem erosiva, foram realizadas as leituras finais. Os resultados obtidos foram submetidos ao teste t, ANOVA e Tukey. As médias de alteração entre os valores de peso finais e iniciais demonstraram diferença significativa (p<0,01) nos materiais estudados e em todos os sucos estudados, com exceção do Vitremer quando imerso no suco de taperebá (p>0,01). As médias de alteração entre os valores de rugosidade superficial final e inicial demonstraram diferença significativa (p<0,01) para todos os materiais estudados em todos os sucos, exceto a Filtek Z350 XT no grupo controle que não apresentou diferença significativa (p>0,01). A comparação entre os valores de microdureza final e inicial demonstrou diferença significativa (p<0,01) na microdureza dos materiais estudados em todos os meios de imersão, inclusive no grupo controle. De um modo geral o suco de taperebá foi o que provocou a maior alteração na superfície dos materiais restauradores quanto ao peso, rugosidade, microdureza e na microscopia eletrônica de varredura. A resina composta Filtek Z350 XT foi o material restaurador que menos sofreu alterações de superfície. Concluiu-se que os sucos das frutas estudados são capazes de alterar os materiais restauradores, sendo que a resina composta foi o material que sofreu menor alteração. / This in vitro study examined the effects of 3 fruit juices with low pH (cupuaçu, taperebá and orange) and artificial saliva (control) upon restorative materials indicated in noncarious cervical lesions: nanoparticle composite resin (Filtek Z350 XT), resin-modified glass ionomer cement (Vitremer) and a glass ionomer cement (Fuji II). The materials were evaluated quantitatively as for alterations in weight, surface roughness and surface microhardness, and qualitatively by scanning electronic microscopy (SEM). 144 specimens were prepared for each quantitative test (n = 12) and 45 for the SEM (n = 3), of (8mm diameter x 2mm height). The specimens were prepared, stored in artificial saliva for 24 hours at 37º C, were finished in a polishing machine, and then the initial readings were performed. During a period of 10 consecutive days, the specimens were subjected to erosive challenge (in the respective juices) for 30 minutes, three times a day, and totaling 90 minutes/day and kept in artificial saliva between intervals. After the erosive cycling period, the final readings were taken. The data were analyzed using t test, ANOVA and Tukey.Test The average alterations between the values of initial and final weight showed significant difference (p < 0.01) in the material studied and all the juices studied, except for Vitremer when immersed in taperebá juice (p > 0.01). The average alterations between the values of initial and final surface roughness showed a significant difference (p < 0.01) for all materials studied in all juices, except for Filtek Z350 XT, in the control group, that showed no significant differences (p > 0.01). The comparison between the values of initial and final microhardness showed a significant difference (p < 0.01) in microhardness of the materials studied in all immersion means, including the control group. In general, taperebá juice was the one that caused the biggest alterations in the surface of restorative materials with respect to weight, roughness, hardness and scanning electronic microscopy. The composite resin Filtek Z350 XT was the restorative material that suffered less surface alterations. It was concluded that the fruit juices studied are capable of altering the restorative materials, and composite resin was the material that has undergone minor changes.

Introdução - A malária é uma das principais doenças humanas do mundo e afeta principalmente as populações pobres em regiões tropicais e subtropicais onde as condições ambientais são favoráveis tanto para a proliferação dos agentes etiológicos como dos mosquitos vetores. No Brasil, An. darlingi é considerado vetor primário de plasmódios humanos. Devido à importância médica, esse inseto tem sido objeto de campanhas de controle populacional. No entanto, não foi considerada a ocorrência de microevolução em An. darlingi e consequentemente, a possibilidade de populações diferentes apresentarem características biológicas distintas. Objetivo Verificar a presença de variabilidade genética e morfológica em populações de An. darlingi no Brasil. Metodologia - Foram analisados e comparados 26 atributos da morfologia externa de ovos de nove populações, bem como a morfometria geométrica da forma alar de espécimes de 10 localidades diferentes de Anopheles darlingi. Além disso, foram empregadas sequências do gene mitocondrial citocromo oxidase subunidade I (COI) para analisar a estrutura populacional de An. darlingi. Resultados e Conclusão Apesar dos atributos dos ovos apresentarem variação, somente as amostras de Tocantins e Pará foram diferenciadas das demais populações. As variações nas estruturas externas dos ovos são provavelmente adaptativas, com influência de fatores ambientais, como temperatura, umidade e disponibilidade de alimento para as fêmeas. A comparação da morfometria geométrica da asa demonstrou que existe maior similaridade entre as populações da costa (estados do Espírito Santo , do cerrado (estados de Goiás e Tocantins), do norte do rio Amazonas (estados do Amazonas e Amapá), e do sul do rio Amazonas (estados de Mato Grosso e Pará). As análises de COI demonstraram diferenciação das populações da costa da Mata Atlântica em relação às demais populações do Brasil central, Amazônia e Mata Atlântica do Interior. O padrão da diversidade de haplótipos de COI, os testes de neutralidade e a distribuição de diferenças pareadas indicaram recente expansão demográfica. A distância geográfica, as ecorregiões e fatores ambietais podem provavelmente limitar a dispersão da espécie, tendo alguma influência sobre a estrutura populacional de An. darlingi / Introduction Malaria is a major human disease that primarily affects poor persons in tropical and subtropical regions where environmental conditions are favorable to the proliferation of the etiological agent as well as vector mosquitoes. In Brazil, Anopheles darlingi is considered a primary vector of human plasmodia and has been the target of control campaigns because of its medical importance. However, the occurrence of microevolution in An. darlingi was not considered and, consequently, the possibility of different populations exhibit distinct biological characteristics. Objective Verify the presence of morphological and genetic variability in Brazilian Anopheles darlingi populations. Methods Twenty six attributes of external egg morphology were analyzed and compared in nine populations. Similarly, the geometric morphometry of wing shape was evaluated in ten An. darlingi localities. In addition, the mitochondrial gene cytochrome oxidase subunit I (COI) was employed to analyze the population structure of An. darlingi. Results and Conclusion - Although, egg attributes showed variation, only samples from Tocantins and Pará were differentiated from other populations. Variation in external egg structure is arguably adaptive in light of environmental factors such as temperature, humidity and food availability for females. Comparisons of wing geometric morphometry indicated that there is greater similarity between Coastal (Espírito Santo and Rio de Janeiro states) and Inner (São Paulo and Paraná states) populations of the Atlantic Forest, and differentiation of those from (Goiás and Tocantins states) and regions both north (Amazonas and Amapá states) and south (Pará and Mato Grosso states) of the Amazon Region. Cytochrome oxidase I analyses indicated differentiation between coastal Atlantic Forest populations (Espírito Santo and Rio de Janeiro states) and those from the cerrado, the Amazon and the interior Atlantic Forest. The pattern of COI haplotype diversity, neutrality tests and distribution of pairwise differences suggest a recent demographic expansion. Geographical distance, ecoregions and potentially environmental constraints may limit the species´ dispersal and influence the population structure of An. darlingi

Plugged and abandoned well pads throughout the Uintah Basin face reclamation challenges due to factors including a harsh climate, invasive species, and high salt loads. Finding ways to alleviate soil sodicity could improve soil reclamation success. Gypsum, sulfur, activated carbon, and Biochar are being applied to improve soil parameters negatively impacted by sodicity, but the direct impact of these amendments on Uintah Basin soils is still largely unknown. The aim of this study was two-fold. (1) Evaluate the effectiveness of gypsum, sulfuric acid, Biochar, activated carbon, and combinations of these amendments in reducing the impact of soil sodicity of the Desilt and Conglomerate soils by measuring amendment impact on percent dispersion, saturated hydraulic conductivity, crust bulk density, infiltration, and crust formation. (2) Compare a crust bulk density method using ImageJ to the clod wax density method and a modified linear extensibility percent equation to the linear extensibility percent equation to assess whether the novel methods can be used to accurately measure and calculate soil crust bulk density and shrink swell potential while reducing human error and analysis time.

The Cold-Gas Dynamic-Spray process also known as Cold Spray (CS) has been researched for three decades. The CS process is a solid-state deposition technique via supersonic velocity of powder particles at a temperature significantly below the melting point of the spray material. This thesis presents background on the overall CS process parameters, and additional information on the microstructural and mechanical properties of typical Cold Sprayed materials.This Thesis primarily presents a study on the microstructural annealing response of CS Al 6061. It should be noted that for this study, the term “annealing” is used in the sense of the classical metallurgical definition of annealing, and not a specific temper designation for the 6061 alloy. Cross sections of CS Al 6061 were imaged with a scanning electron microscope (SEM) in secondary electron (SE), backscatter electron (BSE), and electron backscatter diffraction (EBSD) imaging mode for quantitative and qualitative information on the grain size and orientation of the CS microstructure. The detailed SE, BSE and EBSD mode images present the grain size and grain orientation of the original powder, as received (AR) state and after heat treating at 200°C for 1 hour, 10 hours, and 100 hours. Three different regions, characterized with distinctly differing microstructures, are labeled as low, medium, and high deformation regions, and their microstructures, and evolving features are discussed. Vickers microhardness testing are performed to examine the differences in hardness values between different heat treatments, and for correlation with the level of deformation and grain refinement in the microstructure. SEM imaging was used in BSE mode to correlate microhardness variation to the different regions within the CS microstructure.

In der vorliegenden Arbeit werden epitaktische BaFe2As2 (Ba122)- Dünnschichten, die auf Spinell-Substraten mit einer Pufferschicht aus Eisen mit gepulster Laserabscheidung hergestellt wurden, durch Transmissions- (TEM) und Rasterelektronenmikroskopie (REM) untersucht. Idealerweise weisen die Ba122-Dünnschichten eine biaxiale Zugdehnung von etwa 2% auf, die zur Supraleitung in ihnen führt. Der Schwerpunkt dieser Arbeit richtet sich auf die Defektanalyse und die Untersuchung des Dehnungszustandes auf Inhomogenitäten. Auf allen Dünnschichten werden Droplets des Targetmaterials beobachtet. Wenn die Höhe der Ba122-Schicht mehr als 60 nm beträgt, erfolgt eine Relaxation der Dehnung durch die Bildung von Rissen. Experimente mit konvergenter Elektronenbeugung in einem TEM sind problematisch, weil der Dehnungszustand durch die Probenpräparation (Krümmung der TEM-Lamelle) beeinflusst wird. Durch die Verwendung hochauflösender Beugung rückgestreuter Elektronen (HREBSD) in einem REM wird gezeigt, dass in allen Ba122-Dünnschichten kleine Orientierungsänderungen des Kristallgitters (≤ 0,2°) und Inhomogenitäten des Dehnungszustandes (≤ 2 × 10-4) auf Längenskalen von wenigen 100 nm oder darunter vorliegen. Auf einer Probe werden teilweise dehnungsrelaxierte Stellen nachgewiesen. Es wird außerdem belegt, dass die Eisenpufferschicht eine sehr wichtige Rolle bei der Realstruktur der Ba122-Schicht spielt. Abschließend wird HREBSD mit konventioneller Auswertung der Beugung rückgestreuter Elektronen (EBSD) verglichen. Dabei wird ermittelt, dass mit großem Aufwand und mit optimalen experimentellen Bedingungen auch durch konventionelle Auswertung der EBSD-Pattern Orientierungsunterschiede mit einer Genauigkeit, die besser ist als 0,1°, gemessen werden können. In der Gegenwart von Probenstellen mit unterschiedlichen Dehnungszuständen ergeben sich jedoch deutliche Abweichungen im Gegensatz zu der exakten Auswertung durch HREBSD.