Submitted by Johnny Rodrigues (johnnyrodrigues@ufcg.edu.br) on 2018-05-22T22:23:47Z No. of bitstreams: 1 KATCILÂNYA MENEZES DE ALMEIDA - TESE PPGEA 2012..pdf: 12015723 bytes, checksum: 89f32aca42c4224f2d2241d72785479c (MD5) / Made available in DSpace on 2018-05-22T22:23:47Z (GMT). No. of bitstreams: 1 KATCILÂNYA MENEZES DE ALMEIDA - TESE PPGEA 2012..pdf: 12015723 bytes, checksum: 89f32aca42c4224f2d2241d72785479c (MD5) Previous issue date: 2012-04 / CNPq / O Brasil possui grande potencial agrícola para produzir óleo vegetal, tanto para fins alimentares como para suprir parte da demanda de energia renovável, porém nos últimos cinco anos tem sido o maior importador de azeite de oliva do mundo, devido aos seus benefícios para a saúde. Neste contexto objetivou-se, com este trabalho, a elaboração de misturas especiais de óleos vegetais para fins alimentícios, com base nos óleos de amendoim, gergelim, maracujá e soja. Os óleos de amendoim e gergelim como alternativa por serem culturas produzidas no Brasil, constituem uma fonte de ácidos graxos e antioxidantes tão pouco explorados na alimentação dos brasileiros, tal como o óleo de maracujá como co-produto, descartado pela indústria de suco e ainda o óleo de soja cuja matéria-prima abundante, tornam o produto acessível aos consumidores de todas as classes sociais. Os óleos de amendoim e gergelim foram extraídos de sementes das cultivares BRS-Havana e BRS-Seda, respectivamente, cedidas pela Embrapa Algodão enquanto o óleo de maracujá foi adquirido no comércio de São Paulo e o de soja no de Campina Grande. As misturas foram elaboradas com base em uma matriz de planejamento experimental e, em seguida, submetidas às análises de composição de ácidos graxos e ensaios físico-químicas (umidade, índice de acidez, índice de iodo, índice de refração, densidade e viscosidade) segundo a metodologia do IAL (2008). As medidas obtidas foram utilizadas para estudar e otimizar a elaboração das misturas de óleos vegetais e como variáveis para predição por espectrometria no infravermelho próximo (NIR) foram utilizados os mínimos quadrados parciais (PLS) como metodologia de calibração multivariada. Os resultados foram submetidos à análise de variância (ANOVA), à análise de variância multivariada (MANOVA), à análise de correlação canónica e à análise de correlação de Pearson, pelo software SAS 9.1.3; na análise de componentes principais (PCA) e regressão por mínimos quadrados parciais (PLS) utilizou-se o software Uncrambler 9.8®. Concluiu-se que a mistura equivalente a 40% de óleo de amendoim, 20% de óleo de gergelim, 20% de óleo de maracujá e 20% de óleo de soja apresentou-se como a melhor mistura para fins alimentares, com base na composição de ácidos graxos. Os métodos de predição por NIR foram eficazes para a estimativa não destrutiva, rápida, de baixo custo e direta, dos ácidos graxos palmítico, esteárico, oleico, linoleico, araquídico e linolênico e para as medidas físico-químicas de densidade, índice de refração, viscosidade, índice de acidez e índice de iodo. / Brazil has great potential to produce vegetable oils as a source of raw materiais for food and energy. But in the last five years has been the largest importer of olive oil in the worid due to its health benefits and wide divulgation. In this context, the aim of this work was the development of special blends of vegetable oils as an alternative to olive oils based on peanut, sesame, soy and passion fruit. The peanut and sesame oils because they are a source of fatty acids and antioxidants in the diet of little explored in Brazil, passion fruit oil as co-product of the juice industry, and soybean oil abundant raw material which makes the product available to consumers of ali social classes. The peanut and sesame oils were extracted from seeds of BRS-Seda and BRS-Havana, while passion fruit oil was purchased commercially of city São Paulo-SP and trade soybean in the city of Campina Grande-PB. The mixtures were prepared based on an array of experimental design and then submitted to analysis of fatty acid composition and physico-chemical (moisture, acid value, iodine value, refractive index, density and viscosity). Moreover, were used as reference variables for prediction via infrared spectroscopy (NIR) using the partial least squares (PLS) and multivariate calibration methodology. The results were subjected to analysis of variance (ANOVA), multivariate analysis of variance (MANOVA), canonical correlation analysis and Pearson correlation analysis by SAS 9.1.3 software, the principal component analysis (PCA) and Partial least squares regression (PLS) was used Uncrambler 9.8 ® softwarlt was concluded that the mixture equivalent to 40% peanut oil, 20% sesame oil, 20% passion fruit oil, and 20% soybean oil was presented as the best mix for food composition based on fatty acids. The prediction by NIR methods were effective for estimating non-destructive, rapid, inexpensive and direct fatty acids palmitic, stearic, oleie, linoleic, linolenic and arachidic and physico-chemical measurements of density, refractive index, viscosity, acid value and iodine value.

Made available in DSpace on 2017-07-10T18:08:14Z (GMT). No. of bitstreams: 1 Paulo Sergio Theodoro.pdf: 1744465 bytes, checksum: 132da5a46d9247da552f8a27ee087fed (MD5) Previous issue date: 2010-02-18 / The aim of this work is devoted to reduction of the environmental impact of galvanic industry effluents. An electro-coagulation (EC) laboratory scale system using iron plates electrodes was studied for the removal of organic and inorganic pollutants as a by-product from the treatment of galvanic process based-platining industry. An EC reactor consisting of a 1,5 L conical container and a set of seven firmly assembled iron electrode plates, which were parallelly arranged to each other and electrically operated in mono-polar mode, was built. A 1.0 cm gap between the anode and cathode plates using a non-conducting horizontal support was chosen in order to operate the EC reactor in a low electrical current range. A long, electrical rotating cilindrical rotor, with 2,7cm blades at the end of it, made in non-conducting material, was used to turn mechanically the effluent around the rotor axis during the EC treatment. In addition, a 225 cm2 active electrode surface area was kept during the whole EC experiments. In order to obtain optimal values of reaction time, electrical current, rotor angular velocity, and initial effluent pH, a central composite rotatable design (CCRD) was applied. A wide range of reaction time (10-60 min), electrical current (0.3-3.0 A), rotor angular velocity (50-300 rpm), and initial efluent pH (3-10) were used, performing a total of 28 runs with 24+2x4 axial points and 4 central points. Physico-chemical parameters such as chemical oxygen demand (COD), color, turbidity, total solids, and metals (Cr, Ni, Zn, and Cu) were used as response variables. The measurements of physico-chemical parameter and metal concentration values in non- and treated waste waters were carried out by applying the Standard Methodology and the Synchrotron Radiation X-Ray Fluorescence (SR-TXRF) technique, respectively. Using the Statistica software, a 95%-significance level (p<0.05) of the predicted models and interaction effects between reactor operating variables on response variables were evaluated using 3-D response surface curves and analysis of variance. With the factorial design was obtained the following optimum conditions of the reactor, 35 minutes for the time of electrolysis, 170 rpm for agitation, 2.2 A for the electric current and 6.5 for pH. Under these conditions the removal of color and turbidity reached 100%, another considerable value was the removal of around 90% of COD and total solids. Moreover, a removal of around 99% of Zn and Cu was obtained, whereas for Cr and Ni obtained a removal of 100%. Finally, the results of technical and economic analysis showed the cost obtained by the treatment, indicating clearly that the method of electro-coagulation is very promising for industrial application. / O presente trabalho tem como objetivo remover os poluentes de um efluente de galvanização, de modo a reduzir o impacto ambiental dos efluentes da indústria galvânica. Para a remoção dos poluentes, orgânicos e inorgânicos, gerado nos processos de galvanização foi aplicada a eletrocoagulação (EC) em escala de laboratório utilizando eletrodos de ferro. Foi construído um reator de EC, constituído por um recipiente cônico com capacidade de 1,5 L e um eletrodo de ferro montado firmemente com seis placas de ferro, que foram dispostas paralelamente com uma distância de 1(um) centímetro, operado em modo mono-polar. O sistema de agitação mecânico foi construído com duas pás de geometria cilíndrica de 2,7 cm e uma haste de 31,5 cm feito com material não condutor acoplado em um motor elétrico. Durante o experimento da EC foi utilizada uma área efetiva de 225 cm2 do eletrodo. A fim de obter valores ideais do tempo de eletrolise, corrente elétrica, agitação e pH inicial do efluente, foi aplicado o planejamento estatístico composto central (DCCR) com fatorial 24+2X4 pontos axiais + 4 ponto centrais, totalizando 28 ensaios experimentais. Os valores aplicados as variáveis independentes foram de 0,3 a 3 A para a corrente, de 10 a 60 min. para o tempo de eletrolise, de 3 a 10 para o pH inicial e agitação como valores entre 50 e 300 rpm. Foram utilizadas como variáveis resposta os parâmetros físico químico tais como, a demanda química de oxigênio (DQO), cor, turbidez, Sólidos totais e concentração dos metais Cr, Ni, Zn e Cu.Todos os parâmetros físico-químicos foram determinados através o Método Padrão para análise de água, enquanto que as concentrações dos metais foram determinadas através da técnica de Fluorescência de Raios X por Reflexão Total, (SR-TXRF). Utilizando o software Statistica, com nível de significância de 95% (p <0,05), os modelos preditos e os efeitos de interação entre as variáveis de operação do reator e as variáveis respostas foram avaliados, utilizando as curvas 3-D de superfície de resposta e a análise de variância. Com o planejamento fatorial foi obtido as seguintes condições ótimas de trabalho do reator, 35 minutos para o tempo de eletrolise, 170 rpm para a agitação, 2,2 A para a corrente elétrica e 6,5 para o pH. Nestas condições a remoção da cor e turbidez alcançaram 100%, outro valor considerável foi a remoção em torno de 90% da DQO e sólidos totais. Além disso, uma remoção em torno de 99% de Zn e Cu também foi obtida, enquanto que para o Cr e Ni obteve-se uma remoção de 100%. Finalmente, os resultados da análise técnico-econômica mostraram o baixo custo obtido pelo tratamento, evidenciando claramente que o método da eletrocoagulação é muito promissor para aplicação industrial.

O tratamento cosmético facial e corporal que emprega o Fango vem sendo muito utilizado em clínicas de estética, com o intuito de melhorar a aparência da pele. A literatura científica carece de informações sobre alguns aspectos desta matéria-prima, como: as condições adequadas para sua coleta, preservando suas características químicas e microbiológicas; as especificações de qualidade da matéria-prima (física, química, microbiológica e toxicológica); e as metodologias analíticas de avaliação. A qualificação do Fango é primordial para o mesmo ser utilizado como matéria-prima de uso cosmético \"tal qual\" na pele ou veiculado em formulações cosméticas, a fim de alcançar a eficácia cosmética e garantir sua segurança de uso. Este trabalho visou a padronização do método de coleta do Fango na fonte e a das seguintes análises: física, físico-química, microbiológica, parasitológica, toxicológica do Fango provindo de Araxá-MG in natura e da lama negra (processada), com intuito de assegurar seu uso qualificado como matéria-prima em formulações cosméticas, uma vez que a literatura científica carece de estudos com este tipo de material. Os resultados obtidos quanto à segurança de uso foram satisfatórios, não ocorrendo a presença de microrganismos patogênicos tais como: Escherichia coli, coliformes fecais e totais, Staphylococcus aureus, Pseudomonas aeruginosa e Candida albicans (antes e depois da maturação), larva migrans e metais pesados. Os demais ensaios realizados para a caracterização do Fango como matéria-prima justificam sua aplicação em produtos cosméticos, como por exemplo, a presença do enxofre com potencial uso em formulações antissépticas e a argila tipo \"caulinita\" em preparações para diminuir a oleosidade da pele. / The facial and body cosmetic treatments applying the \"Fango\" can be seen nowadays on esthetic clinics\' catalogues. The scientific literature up nowadays does not have sufficient informations concerning this product, the correct procedures to collect it from the soil preserving its chemical and microbiological characteristics; the specifications on its physical, chemical, microbiological e toxicological qualities and the analytical methodologies involving on the it evaluation. The Fango\'s qualification is very important because it can be used alone (raw material) or incorporated in cosmetic formulations, in order to evaluate the safety and efficacy of final product. This is the only way it may be applied on cosmetics formulations designed to be applied on human skin. The aim of this research is to standard the collect conditions in thermal springs and standard such analysis: physical aspects, physic-chemical, microbiology, parasitological and toxicological of Thermal mud and Fango from Araxá-MG. The results obtained of this study showed that the Fango from Araxá-MG is safe to be applied in cosmetic formulations or direct on the human skin. The pathogenic microorganism such as: Escherichia coli, Staphylococcus aureus, Pseudomonas aeuruginosa and Candida Albicans were absent on the samples, and the same to Larva migrans and heavy metais. The physic-chemical analysis of Fango from Araxá-MG demonstrated its application in cosmetic products, as its capacity to improvement the skin\'s conditions, e.g. the presence of sulphur with antiseptic proprieties and organic compounds in order to use on the oily skin.

Deep geological repository (DGR) for disposal of high-level radioactive waste (HLW) is designed to rely on successive superimposed barrier systems to isolate the waste from the biosphere. This multiple barrier system comprises the natural geological barrier provided by the repository host rock and its surrounding and an engineered barrier system (EBS). The EBS represents the synthetic, engineered materials placed within the natural barrier, comprising array of components such as waste form, waste canisters, buffer materials, backfill and seals. The buffer will enclose the waste canisters from all directions and act as a barrier between canisters and host rock of the repository. It is designed to stabilise the evolving thermo-hydro-mechanical-chemical stresses in the repository over a long period (nearly 1000 years) to retard radionuclides from reaching biosphere. Bentonite clay or bentonite-sand mix have been chosen as buffer materials in EBS design in various countries pursuing deep geological repository method. The bentonite buffer is the most important barrier among the other EBS components for a geological repository. The safety of repository depends to a large extent on proper functioning of buffer over a very long period of time during which it must remain physically, chemically and mineralogically stable. The long term stability of bentonite buffer depends on varying temperature and evolution of groundwater composition of host rocks in a complex way. The groundwater in the vicinity of deep crystalline rock is often characterized by high solute concentrations and the geotechnical engineering response of bentonite buffer could be affected by the dissolved salt concentration of the inflowing ground water. Also during the initial period, radiogenic heat produced in waste canisters would radiate into buffer and the heat generated would lead to drying and some shrinkage of bentonite buffer close to canister. This could alter the dry density, moisture content and in turn the hydro-mechanical properties of bentonite buffer in DGR conditions. India has variety of bentonite deposits in North-Western states of Rajasthan and Gujarat. Previous studies on Indian bentonites suggest that bentonite from Barmer district of Rajasthan (termed as Barmer-1 bentonite) is suitable to serve as buffer material in DGR conditions. Nuclear power agencies of several countries have identified suitable bentonites for use as buffer in DGR through laboratory experiments and large scale underground testing facilities. Physico-chemical, mineralogical and engineering properties of Kunigel VI, Kyungju, GMZ, FoCa clay, MX-80, FEBEX and Avonseal bentonites have been extensively studied by Japan, South Korea, China, Belgium, Sweden, Spain, Canada. It is hence essential to examine the suitability of Barmer-1 bentonite as potential buffer in DGR and compare its physico-chemical and hydromechanical properties with bentonite buffers identified by other countries. The significant factors that impact the long-term stability of bentonite buffer in DGR include variations in moisture content, dry density and pore water chemistry. With a view to address these issues, the hydromechanical response of 70 % Barmer-1 bentonite + 30 % river sand mix (termed bentonite enhanced sand, BES specimens) under varying moisture content, dry density and pore water salt concentration conditions have been examined. The broad scope of the work includes: 1) Characterise the physico-chemical and hydro-mechanical properties of Barmer-1 bentonite from Rajasthan, India and compare its properties with bentonite buffers reported in literature. 2) Examine the influence of variations in dissolved salt concentration (of infiltrating solution), dry density and moisture content of compacted BES specimens on their hydro-mechanical response; the hydro-mechanical properties include, swell pressure, soil water characteristic curve (SWCC), unsaturated hydraulic conductivity, moisture diffusivity and unconfined compression strength. Organization of thesis: After the first introductory chapter, a detailed review of literature is performed to highlight the need for detailed characterisation of physico-chemical and hydromechanical properties of Barmer-1 bentonite for its possible application in DGR in the Indian context. Further, existing literature on hydro-mechanical response of bentonite buffer to changes in physical (degree of saturation/moisture content, dry density) and physico-chemical (solute concentration in pore water) is reviewed to define the scope and objectives of the present thesis in Chapter 2. Chapter 3 presents a detailed experimental programme of the study. Chapter 4 characterises Barmer-1 bentonite for physico-chemical (cation exchange capacity, pore water salinity, exchangeable sodium percentage) and hydro-mechanical properties, such as, swell pressure, saturated permeability, soil water characteristic curve (SWCC) and unconfined compression strength. The properties of Barmer-1 bentonite are compared with bentonite buffers reported in literature and generalized equations for determining swell pressure and saturated permeability coefficient of bentonite buffers are arrived at. Chapter 5 describes a method to determine solute concentrations in the inter-lamellar and free-solutions of compacted BES (bentonite enhanced sand) specimens. The solute concentrations in micro and macro pore solutions are used to examine the role of osmotic flow on swell pressures developed by compacted BES specimens (dry density 1.50-2.00 Mg/m3) inundated with distilled water and NaCl solutions (1000-5000 mg/L). The number of hydration layers developed by the compacted BES specimens on inundation with salt solutions in constant volume swell pressure tests is controlled by cation hydration/osmotic flow. The cation hydration of specimens compacted to dry density of 2.00 Mg/m3 is mainly driven by matric suction prevailing in the clay microtructure as the number of hydration layers developed at wetting equilibrium are independent of the total dissolved solids (TDS) of the wetting solution. Consequently, the swell pressures of specimens compacted to 2.00 Mg/m3 were insensitive to the salt concentration of the inundating solution. The cation hydration of specimens compacted to dry density of 1.50 Mg/m3 is driven by both matric suction (prevailing in the clay micro-structure) and osmotic flow as the number of hydration layers developed at wetting equilibrium is sensitive to the TDS of the wetting solution. Expectedly, the swell pressures of specimens compacted to 1.50 Mg/m3 responded to changes in salt concentration of the inundating solution. The 1.75 Mg/m3 specimens show behaviour that is intermediate to the 1.50 and 2.00 Mg/m3 series specimens. Chapter 6 examines the influence of initial degree of saturation on swell pressures developed by the compacted BES specimens (dry density range: 1.40- 2.00 Mg/m3) on wetting with distilled water from micro-structural considerations. The micro-structure of the bentonite specimens are examined in the compacted and wetted states by performing X-ray diffraction measurements. The initial degree of saturation is varied by adding requisite amount of distilled water to the oven-dried BES mix and compacting the moist mixes to the desired density. The montmorillonite fraction in the BES specimens is responsible for moisture absorption during compaction and development of swell pressure in the constant volume oedometer tests. Consequently, it was considered reasonable to calculate degree of saturation based on EMDD (effective montmorillonite dry density) values and correlate the developed swell pressure values with degree of saturation of montmorillonite voids (Sr,MF). XRD measurements with compacted and wetted specimens demonstrated that if specimens of density series developed similar number of hydration layers on wetting under constant volume condition they exhibited similar swell pressures, as was the case for specimens belonging to 1.40 and 1.50 Mg/m3 series. With specimens belonging to 1.75 and 2.00 Mg/m3 series, greater number of hydration layers were developed by specimens that were less saturated initially (smaller initial Sr,MF) and consequently such specimens developed larger swell pressures. When specimens developed similar number of hydration layers in the wetted state, the compaction dry density determined the swell pressure. Chapter 7 examines the influence of salt concentration of infiltrating solution (sodium chloride concentration ranges from 1000- 5000 mg/L) on SWCC relations, unsaturated permeability and moisture diffusivity of compacted BES specimens. Analysis of the experimental and Brooks and Corey best fit plots revealed that infiltration of sodium chloride solutions had progressively lesser influence on the micro-structure and consequently on the SWCC relations with increase in dry density of the compacted specimens. The micro-structure and SWCC relations of specimens compacted to 1.50 Mg/m3 were most affected, specimens compacted to 1.75 Mg/m3 were less affected, while specimens compacted to 2.00 Mg/m3 were unaffected by infiltration of sodium chloride solutions. Variations in dry density of compacted bentonite impacts the pore space available for moisture flow, while, salinity of wetting fluid impacts the pore structure from associated physico-chemical changes in clay structure. Experimental results showed that the unsaturated permeability coefficient is insensitive to variations in dry density and solute concentration of wetting liquid, while, the effective hydraulic diffusivity is impacted by variations in these parameters. Chapter 8 summarises the major findings of the study.

Deep geological repository (DGR) for disposal of high-level radioactive waste (HLW) is designed to rely on successive superimposed barrier systems to isolate the waste from the biosphere. This multiple barrier system comprises the natural geological barrier provided by the repository host rock and its surrounding and an engineered barrier system (EBS). The EBS represents the synthetic, engineered materials placed within the natural barrier, comprising array of components such as waste form, waste canisters, buffer materials, backfill and seals. The buffer will enclose the waste canisters from all directions and act as a barrier between canisters and host rock of the repository. It is designed to stabilise the evolving thermo-hydro-mechanical-chemical stresses in the repository over a long period (nearly 1000 years) to retard radionuclides from reaching biosphere. Bentonite clay or bentonite-sand mix have been chosen as buffer materials in EBS design in various countries pursuing deep geological repository method. The bentonite buffer is the most important barrier among the other EBS components for a geological repository. The safety of repository depends to a large extent on proper functioning of buffer over a very long period of time during which it must remain physically, chemically and mineralogically stable. The long term stability of bentonite buffer depends on varying temperature and evolution of groundwater composition of host rocks in a complex way. The groundwater in the vicinity of deep crystalline rock is often characterized by high solute concentrations and the geotechnical engineering response of bentonite buffer could be affected by the dissolved salt concentration of the inflowing ground water. Also during the initial period, radiogenic heat produced in waste canisters would radiate into buffer and the heat generated would lead to drying and some shrinkage of bentonite buffer close to canister. This could alter the dry density, moisture content and in turn the hydro-mechanical properties of bentonite buffer in DGR conditions. India has variety of bentonite deposits in North-Western states of Rajasthan and Gujarat. Previous studies on Indian bentonites suggest that bentonite from Barmer district of Rajasthan (termed as Barmer-1 bentonite) is suitable to serve as buffer material in DGR conditions. Nuclear power agencies of several countries have identified suitable bentonites for use as buffer in DGR through laboratory experiments and large scale underground testing facilities. Physico-chemical, mineralogical and engineering properties of Kunigel VI, Kyungju, GMZ, FoCa clay, MX-80, FEBEX and Avonseal bentonites have been extensively studied by Japan, South Korea, China, Belgium, Sweden, Spain, Canada. It is hence essential to examine the suitability of Barmer-1 bentonite as potential buffer in DGR and compare its physico-chemical and hydromechanical properties with bentonite buffers identified by other countries. The significant factors that impact the long-term stability of bentonite buffer in DGR include variations in moisture content, dry density and pore water chemistry. With a view to address these issues, the hydromechanical response of 70 % Barmer-1 bentonite + 30 % river sand mix (termed bentonite enhanced sand, BES specimens) under varying moisture content, dry density and pore water salt concentration conditions have been examined. The broad scope of the work includes: 1) Characterise the physico-chemical and hydro-mechanical properties of Barmer-1 bentonite from Rajasthan, India and compare its properties with bentonite buffers reported in literature. 2) Examine the influence of variations in dissolved salt concentration (of infiltrating solution), dry density and moisture content of compacted BES specimens on their hydro-mechanical response; the hydro-mechanical properties include, swell pressure, soil water characteristic curve (SWCC), unsaturated hydraulic conductivity, moisture diffusivity and unconfined compression strength. Organization of thesis: After the first introductory chapter, a detailed review of literature is performed to highlight the need for detailed characterisation of physico-chemical and hydromechanical properties of Barmer-1 bentonite for its possible application in DGR in the Indian context. Further, existing literature on hydro-mechanical response of bentonite buffer to changes in physical (degree of saturation/moisture content, dry density) and physico-chemical (solute concentration in pore water) is reviewed to define the scope and objectives of the present thesis in Chapter 2. Chapter 3 presents a detailed experimental programme of the study. Chapter 4 characterises Barmer-1 bentonite for physico-chemical (cation exchange capacity, pore water salinity, exchangeable sodium percentage) and hydro-mechanical properties, such as, swell pressure, saturated permeability, soil water characteristic curve (SWCC) and unconfined compression strength. The properties of Barmer-1 bentonite are compared with bentonite buffers reported in literature and generalized equations for determining swell pressure and saturated permeability coefficient of bentonite buffers are arrived at. Chapter 5 describes a method to determine solute concentrations in the inter-lamellar and free-solutions of compacted BES (bentonite enhanced sand) specimens. The solute concentrations in micro and macro pore solutions are used to examine the role of osmotic flow on swell pressures developed by compacted BES specimens (dry density 1.50-2.00 Mg/m3) inundated with distilled water and NaCl solutions (1000-5000 mg/L). The number of hydration layers developed by the compacted BES specimens on inundation with salt solutions in constant volume swell pressure tests is controlled by cation hydration/osmotic flow. The cation hydration of specimens compacted to dry density of 2.00 Mg/m3 is mainly driven by matric suction prevailing in the clay microtructure as the number of hydration layers developed at wetting equilibrium are independent of the total dissolved solids (TDS) of the wetting solution. Consequently, the swell pressures of specimens compacted to 2.00 Mg/m3 were insensitive to the salt concentration of the inundating solution. The cation hydration of specimens compacted to dry density of 1.50 Mg/m3 is driven by both matric suction (prevailing in the clay micro-structure) and osmotic flow as the number of hydration layers developed at wetting equilibrium is sensitive to the TDS of the wetting solution. Expectedly, the swell pressures of specimens compacted to 1.50 Mg/m3 responded to changes in salt concentration of the inundating solution. The 1.75 Mg/m3 specimens show behaviour that is intermediate to the 1.50 and 2.00 Mg/m3 series specimens. Chapter 6 examines the influence of initial degree of saturation on swell pressures developed by the compacted BES specimens (dry density range: 1.40- 2.00 Mg/m3) on wetting with distilled water from micro-structural considerations. The micro-structure of the bentonite specimens are examined in the compacted and wetted states by performing X-ray diffraction measurements. The initial degree of saturation is varied by adding requisite amount of distilled water to the oven-dried BES mix and compacting the moist mixes to the desired density. The montmorillonite fraction in the BES specimens is responsible for moisture absorption during compaction and development of swell pressure in the constant volume oedometer tests. Consequently, it was considered reasonable to calculate degree of saturation based on EMDD (effective montmorillonite dry density) values and correlate the developed swell pressure values with degree of saturation of montmorillonite voids (Sr,MF). XRD measurements with compacted and wetted specimens demonstrated that if specimens of density series developed similar number of hydration layers on wetting under constant volume condition they exhibited similar swell pressures, as was the case for specimens belonging to 1.40 and 1.50 Mg/m3 series. With specimens belonging to 1.75 and 2.00 Mg/m3 series, greater number of hydration layers were developed by specimens that were less saturated initially (smaller initial Sr,MF) and consequently such specimens developed larger swell pressures. When specimens developed similar number of hydration layers in the wetted state, the compaction dry density determined the swell pressure. Chapter 7 examines the influence of salt concentration of infiltrating solution (sodium chloride concentration ranges from 1000- 5000 mg/L) on SWCC relations, unsaturated permeability and moisture diffusivity of compacted BES specimens. Analysis of the experimental and Brooks and Corey best fit plots revealed that infiltration of sodium chloride solutions had progressively lesser influence on the micro-structure and consequently on the SWCC relations with increase in dry density of the compacted specimens. The micro-structure and SWCC relations of specimens compacted to 1.50 Mg/m3 were most affected, specimens compacted to 1.75 Mg/m3 were less affected, while specimens compacted to 2.00 Mg/m3 were unaffected by infiltration of sodium chloride solutions. Variations in dry density of compacted bentonite impacts the pore space available for moisture flow, while, salinity of wetting fluid impacts the pore structure from associated physico-chemical changes in clay structure. Experimental results showed that the unsaturated permeability coefficient is insensitive to variations in dry density and solute concentration of wetting liquid, while, the effective hydraulic diffusivity is impacted by variations in these parameters. Chapter 8 summarises the major findings of the study.

En Europe, suite à la fermeture de nombreux sites sidérurgiques, une utilisation croissante de laitiers de haut-fourneau d’origine et d’âge variés voit le jour depuis plusieurs années. Cette évolution conduit à une diversification de la composition chimique et minéralogique des laitiers. Connaître l’influence de ces caractéristiques sur la réactivité des laitiers utilisés en substitution du clinker dans les ciments de haut-fourneau (CEM III) devient, dès lors, primordial pour assurer les performances de tels ciments.<p><p>Dans ce contexte, le présent travail a pour but d’investiguer l’influence de la composition chimique et de l’âge des laitiers sur leur réactivité tant par des essais physico-mécaniques que par une caractérisation physico-chimique et minéralogique de CEM III/B à différentes échéances d’hydratation. L’effet néfaste du vieillissement des laitiers est clairement mis en exergue et son impact diffère selon la composition chimique de départ du laitier. Les ions aluminium engendrent une accélération de l’hydratation et une amélioration des résistances physico-mécaniques à jeune âge mais, à long terme, ils conduisent à une perte de ces dernières. Concernant l’influence des ions titane dans les laitiers, la tendance générale observée est une diminution des performances physico-mécaniques.<p><p>Sur base de ces résultats, une évaluation de la représentativité de moyens accélérés d’estimation de la réactivité des laitiers est effectuée. Il est mis en évidence que seules les mesures de résistances physico-mécaniques classiques permettent d’évaluer correctement la réactivité des différents laitiers.<p><p>Une évaluation de la détermination de la teneur en constituants de CEM III/B par la méthode Rietveld est menée par comparaison avec la méthode de dissolution sélective de la norme EN 196-4 et le dosage des constituants par pesée. Moyennant une utilisation adaptée de cette méthode, les résultats obtenus à l’aide de celle-ci sont très encourageants.<p><p><p>In Europe, following the closure of many steel plants, an increased use of blast furnace slag (BFS) of various age and origin was born for several years. This evolution leads to a diversification of the chemical and mineralogical composition of the BFS. Knowing the influence of these characteristics on the reactivity of slag used in substitution of clinker in blast-furnace cement (CEM III) becomes, therefore, crucial to ensure the performance of such cements. <p><p>In this context, this work aims to investigate the influence of chemical composition and age of BFS on their reactivity by both physico-mechanical and physico-chemical and mineralogical characterization of CEM III/B at different times of hydration. The adverse effect of ageing of BFS is clearly highlighted and its impact varies depending on the chemical composition of the BFS. Aluminum ions generate an acceleration of the hydration and improve mechanical strength at early age, but at long term, they lead to a loss of the strength. Regarding the influence of titanium ions in the BFS, the general trend is a decrease of the physical and mechanical performance.<p><p>Based on these results, an assessment of the representativeness of accelerated means of estimating, the BFS reactivity is done. It is emphasized that only measures of physical and conventional mechanical strength can accurately assess the reactivity of different BFS. <p><p>An evaluation of the determination of the amount of CEM III/B components by the Rietveld method is based upon comparison with the selective dissolution method from the EN 196-4 norm and components determination by weight. Through appropriate use of this method, the results obtained are very encouraging.<p> / Doctorat en Sciences / info:eu-repo/semantics/nonPublished

Le but de ce travail est d’étudier le potentiel d’un bitume naturel (BN) extrait en Albanie pour la production des bitumes durs (BD) et des enrobés à module élevé (EME). Pour la production des BD, différentes techniques de raffinage du pétrole existent. Néanmoins, avec certains bruts pétroliers il est impossible de les fabriquer. De plus, les BD de raffinerie comportent souvent des défauts qui limitent leurs applications. Ces raisons, couplées à des questions d’approvisionnement, conduisent à chercher des méthodes de substitution. Dans ce contexte, il est intéressant d’utiliser des BN. Cette étude a montré que le BN d’Albanie donne des BD et des EME en conformité avec la Normalisation Européenne, résistants au vieillissement et performants aux basses températures. Un dosage adéquat permet de formuler des matériaux d’une dureté désirée en réponse des exigences techniques des applications routières visées tout en facilitant la gestion des stocks de bitumes dans les centrales d’enrobages. / The aim of this thesis is to study the potential of a natural bitumen (NB) mined in Albania in the production of hard bitumens (HB) and that of high modulus asphalt concrete (HMAC). Various petroleum refining techniques are available for the production of HB. Nevertheless, this is impossible with some crude oils. In addition, HB from refineries often present shortcomings which limit their applications. These reasons, coupled with practical issues related to HB supply, motivate the research of alternative methods. In this industrial context it is interesting to use NB. This study has shown that the Albanian NB provides HB and HMAC in accordance with European Standards, resistant to aging and relatively performant at low temperatures. The proper dosage of this NB allows the formulation of materials of desired properties, in response to the technical requirements of the considered road applications, facilitating in this way the use of bitumen stocks in asphalt concrete production plants.

O mel é um alimento de uso milenar, açucarado de fácil digestão, que constitui uma importante fonte de energia, contribuindo para o equilíbrio do processo biológico do corpo humano, sendo elaborado a partir da desidratação e transformação do néctar das flores nativas pelas abelhas produtoras. Para que o mel seja comercializado para o consumo humano, ele precisa atender aos requisitos mínimos de identidade e qualidade exigidos pela Legislação Brasileira. No Brasil a criação de abelhas é dividida em duas práticas distintas, a Apicultura tradicional, que utiliza as abelhas Apis mellifera e a Meliponicultura que utiliza as abelhas sem ferrão como a Jataí (Tetragonisca angustula). Os méis de abelhas sem ferrão tem maior valor comercial comparado ao mel tradicional, entretanto são comercializados sem uma legislação própria. Na literatura existem poucos trabalhos que tratam da composição destes tipos de méis que são popularmente conhecidos por suas propriedades benéficas à saúde. Em vista do exposto acima, o objetivo deste presente trabalho foi o de comparar a composição e a qualidade de méis de Apis mellifera com os de abelhas sem ferrão da espécie Tetragonisca angustula, popularmente conhecida como Jataí. Para tanto as amostras de méis foram obtidas de colméias de Apis mellifera e de Tetragonisca angustula de uma mesma região botânica, o que foi possível constatar que os méis de abelha Jataí apresentaram maior diversidade botânica em relação aos méis de Apis. Neste trabalho foram utilizados os métodos de avaliação estabelecidos pela Legislação Brasileira para qualidade de mel de Apis mellifera e os valores sugeridos para méis de mellponíneos do Brasil pe10s pesquisadores VILLAS - BOAS e MALASPINA (2005). A maioria das amostras de Apis apresentaram-se dentro da legislação vigente, enquanto méis Jataí apresentaram os parâmetros: umidade (23,40 -25,60%), acidez (21,65 - 63,85 mE/Kg) e açúcares redutores (44,78 - 67,54%) e sacarose aparente (0,43 - 1,60%) fora dos padrões estabelecido pela legislação vigente para os méis de Apis mellifera. No entanto, encontram-se dentro dos valores sugeridos para méís de meliponíneos brasileiros, pelos pesquisadores acima mencionados. Além das análises físico-químicas tradicionais e a análise polínica também foi determinada a composição nutricional, sendo que o mel de Apis apresentou maior de valor energético (43,58- 66,32 Kcal) em relação aos méis de Jataí (36,83 - 60,52 Kcal) (p<0,05). Também foram determinados os açúcares por CLAE, condutividade elétrica (uS/cm-1) e a análise de cor (mmPfund). As amostras de Apis mellifera apresentaram maior o teor glicose (%), frutose (%) e condutividade elétrica (uS/cm-1) em relação aos méis de Jataí Em relação as análises de cor notou-se maior predominância da coloração âmbar-claro, mas amostras analisadas. / Honey is considered as a food that provides energy, being elaborated from the dehydration and transformation of the nectar of the flowers by the bees. For the human consumption, honey needs to attend the minimum requirements of identity and quality demanded by the regulation. In Brazil beekeepers can be divided in two practical distinct ones: the traditional ones, which use Apis mellifera bees and the Meliponiculture which uses stingless bees such as Jataí bee (Tetragonisca angustula). There are no identity and quality parameters or regulation for this type of honey. Honey from of stingless bees are more expensive compared with the traditional honey, however their are commercialized without a proper regulation. In literature few works were found regarding the composition of these types of honey which are popularly known by its beneficiaI properties to human health. The objective of the present work is to compare the composition and quality of honey from Apis mellifera and from stingless bees (Tetragonisca angustula), popularly known as Jataí bee. Samples of honey were obtained from Apis mellifera and Tetragonisca angustula bees in the same botanical region. In this work the methods used were based on the Brazilian Regulation for quality control of honey from Apis mellifera and the values suggested for honeys of meliponíneos of Brazil for researchers VILLAS-BOAS and MALASPINA (2005). The majority of the samples of Apis had presented in accordance with the regulation while the Jataí honeys had presented: humidity (23,40 - 25.60%), acidity (21,65 - 63,85 mE/Kg) and reducing sugars (44,78 - 67.54%) are out of the standards for honeys of Apis mellifera. However, they are in accordance with the values suggested for honeys of Brazilian meliponíneos. The physicochemical, polinic and nutritional analysis were determined, and the honey of Apis bee presented greater amount of energy value (43,58 - 66,32 Kcal) in relation to the honeys of Jataí bee (36,83 - 60,52 Kcal) (p<O,05). The sugars for HPLC, electric conductivity (uS/cm-1) and analysis of color (mmPfund) were determined. Samples of Apis mellifera had presented greater values for glucose (%), frutose (%) and electric conductivity (uS/cm-1) in relation to the honeys from Jataí (p<0,05). Regarding the color analyses, it was predominance of the coloration clear -amber.

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The diploma thesis is focused on fire-resistant repair mortar with fine-grained filler. The aim of this work is the research and development of fine-grained Mortars resistant to high temperatures, which are characteristic at the beginning of the fire. The theoretical knowledge with subsequently realized laboratory verification was used. At-tention was paid to the masses based on the mixed binder comprising cement and blast furnace slag, respectively. high-temperature ash. Cellulose fibres were used as the dis-persed reinforcement. Two kinds of aggregate were assessed - fly ash agloporit and am-phibolite incl. combinations thereof. Laboratory tests were carried out via determination of basic material properties (density, strength, consistency, dimensional changes etc.) after exposure to extreme temperatures. A substantial part of the research was also study of different cooling conditions - slow and fast (water and air). Selected formulations were subjected to temperatures up to 1200 ° C. In the conclusion is selected several recipes that have been found to be optimal for continuing research on the basis of the results and findings.