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In recent years gasoline engines have become increasingly complex, for example through the introduction of electronic control and monitoring systems for ignition, fuel injection and exhaust aftertreatment. Parallel to this the requirements placed upon engines have also increased hence the need to develop new engine technologies. This demand for new technologies is, in part, due to the self obligation of the automobile industry to reduce the CO2 emissions about 25% by 2005, and also to the increasingly stringent future exhaust limits. Some promising solutions are currently in development, e.g. the direct injection gasoline engine and variable valve trains. All these new technologies are characterised by increasing complexity and significantly higher degrees of freedom. The associated application expenditure rises drastically with the number of free parameters and also with improved quality standards. Possible solutions to meet the future requirements of the development process are based on model-based parameter optimisation and the use of test methods, such as "Design of Experiments" (DoE). The idea behind this approach is to produce models to describe the dependence of the responses of interest (i.e. fuel consumption) on the adjusted engine parameters. With these models offline optimisation of the engine can be carry out, independently of testbench resources. The measured data for the models are produced with the help of statistically designed experiments. Thus, the testing and analysis processes are structured and the expenditure limited. In the following the DoE methodology will be employed of a gasoline engine with electromechanical valve train. / Der Ottomotor im Kraftfahrzeug hat in den letzten Jahren mit dem Einzug elektronischer Steuer- und Regelsysteme für Zündung, Einspritzung und Abgasnachbehandlung einen sehr hohen technischen Stand erreicht. Die wachsenden Ansprüche an die Motorenentwicklung im Hinblick auf Verbrauchsreduzierung bei gleichzeitiger Erfüllung der zukünftigen Abgasgrenzwerte, verschärfen den Druck zur Entwicklung weiterführender Technologien. Hierbei gibt es bereits einige vielversprechende Lösungsansätze, wie z.B. die Direkteinspritzung oder variable Ventilsteuerungen. All diese neuen Technologien zeichnen sich durch eine wachsende Komplexität durch die signifikant höhere Anzahl von Freiheitsgraden aus. Der damit verbundene Applikationsaufwand steigt drastisch durch die wachsende Anzahl freier Parameter, aber auch durch die steigenden Anforderungen an die Qualität der Applikationsergebnisse. Einen möglichen Lösungsansatz zur Realisierung der zukünftigen Anforderungen an den Entwicklungsprozess stellen die modellgestützte Parameteroptimierung sowie der Einsatz der "Statistischen Versuchsplanung" (SVP) - "Design of Experiments" (DoE) - dar. Der Grundgedanke basiert auf der Erstellung von Modellen zur Beschreibung der Abhängigkeiten variierter Verstellparameter. Mit diesen Modellen können Offline-Optimierungen unabhängig von Prüfstandsressourcen durchgeführt werden. Die für die Modellbildung benötigten Messdaten werden mit Hilfe der statistischen Versuchsplanung erzeugt. Dadurch wird der Prozess strukturiert und der Aufwand wird begrenzt. In der Arbeit wird der Einsatz der DoE-Methodik am Beispiel eines Ottomotors mit elektromechanischer Ventilsteuerung (EMVS) aufgezeigt.

In recent years gasoline engines have become increasingly complex, for example through the introduction of electronic control and monitoring systems for ignition, fuel injection and exhaust aftertreatment. Parallel to this the requirements placed upon engines have also increased hence the need to develop new engine technologies. This demand for new technologies is, in part, due to the self obligation of the automobile industry to reduce the CO2 emissions about 25% by 2005, and also to the increasingly stringent future exhaust limits. Some promising solutions are currently in development, e.g. the direct injection gasoline engine and variable valve trains. All these new technologies are characterised by increasing complexity and significantly higher degrees of freedom. The associated application expenditure rises drastically with the number of free parameters and also with improved quality standards. Possible solutions to meet the future requirements of the development process are based on model-based parameter optimisation and the use of test methods, such as "Design of Experiments" (DoE). The idea behind this approach is to produce models to describe the dependence of the responses of interest (i.e. fuel consumption) on the adjusted engine parameters. With these models offline optimisation of the engine can be carry out, independently of testbench resources. The measured data for the models are produced with the help of statistically designed experiments. Thus, the testing and analysis processes are structured and the expenditure limited. In the following the DoE methodology will be employed of a gasoline engine with electromechanical valve train. / Der Ottomotor im Kraftfahrzeug hat in den letzten Jahren mit dem Einzug elektronischer Steuer- und Regelsysteme für Zündung, Einspritzung und Abgasnachbehandlung einen sehr hohen technischen Stand erreicht. Die wachsenden Ansprüche an die Motorenentwicklung im Hinblick auf Verbrauchsreduzierung bei gleichzeitiger Erfüllung der zukünftigen Abgasgrenzwerte, verschärfen den Druck zur Entwicklung weiterführender Technologien. Hierbei gibt es bereits einige vielversprechende Lösungsansätze, wie z.B. die Direkteinspritzung oder variable Ventilsteuerungen. All diese neuen Technologien zeichnen sich durch eine wachsende Komplexität durch die signifikant höhere Anzahl von Freiheitsgraden aus. Der damit verbundene Applikationsaufwand steigt drastisch durch die wachsende Anzahl freier Parameter, aber auch durch die steigenden Anforderungen an die Qualität der Applikationsergebnisse. Einen möglichen Lösungsansatz zur Realisierung der zukünftigen Anforderungen an den Entwicklungsprozess stellen die modellgestützte Parameteroptimierung sowie der Einsatz der "Statistischen Versuchsplanung" (SVP) - "Design of Experiments" (DoE) - dar. Der Grundgedanke basiert auf der Erstellung von Modellen zur Beschreibung der Abhängigkeiten variierter Verstellparameter. Mit diesen Modellen können Offline-Optimierungen unabhängig von Prüfstandsressourcen durchgeführt werden. Die für die Modellbildung benötigten Messdaten werden mit Hilfe der statistischen Versuchsplanung erzeugt. Dadurch wird der Prozess strukturiert und der Aufwand wird begrenzt. In der Arbeit wird der Einsatz der DoE-Methodik am Beispiel eines Ottomotors mit elektromechanischer Ventilsteuerung (EMVS) aufgezeigt.

This thesis deals with choises of using mathematical statistics when optimising the compression casting process of high-voltage device transformer. There is a theoretical consideration to be found in the introduction which concerns the compression casting itself and all necessary information connected with it. Then there is a key numerical analysis part following. In the first instance there are variability problems of individual casting device discussed and then a regression analysis made to demonstrate and prove a link between the partial discharge and the key parameters of casting process. Finally an “optimal” casting sequence is suggested and alternative attitude problems with the assistance of Design of Experiments (DOE) are discussed.

Friction Stir Welding (FSW) was used to perform Bead on Plate (BOP) welds on 6061-T6511 aluminum extrusions. Using a DOE approach, tool rotation speed, clamp spacing, and clamping force were altered to ascertain their effects on distortion in the welded panels. Mechanical forces were monitored during the weld process. Both linear and out of plane distortion were measured on the welded extrusions. The Vickers hardness of the weld nugget was measured. The effect of each parameter on weld distortion was discovered and the mechanism of this link was suggested.

No caso de indústrias que utilizam processos de tingimento, a remoção da cor dos seus efluentes líquidos é uma grande preocupação. Os corantes azóicos representam 60% dos corantes utilizados na atualidade em todo o mundo; no entanto, são conhecidos pelo seu efeito carcinogênico e mutagênico, tornando-se urgente o seu tratamento. Assim sendo, tem surgido diversas alternativas aos processos convencionais de tratamento, relativamente aos processos de tratamento de efluentes convencionais, notadamente o processo Fenton, que se tem mostrado bastante promissor. Neste trabalho, investigou-se a otimização do processo Fenton, relativamente ao descoramento de dois corantes azóicos: a azorubina (C20H12N2Na2O7S2, C.I. 14720) e a tartrazina (C16H7N4Na3O9S2, C.I. 19140). Para tal, realizou-se um planejamento composto central, ajustou-se um modelo polinomial (empírico) aos dados experimentais obtidos e obtiveram-se as condições ótimas: razão [Fe2+]/[H2O2] = 0,64 e 0,32, pH = 1,5 e 2,8 e temperatura = 39°C. As variáveis-resposta foram: o grau de descoramento (medido pela área sob o espectro na região do visível) e as concentrações residuais de H2O2 (método do vanadato) e Fe (método da o-fenantrolina). Determinou-se o grau de mineralização por análises de carbono orgânico dissolvido e também a fitotoxicidade a sementes de alface (Lactuca sativa). Realizaram-se análises por CLAE-DAD de forma a se observar a geração dos produtos de oxidação. Obtiveram-se descoramentos de aproximadamente 100% para os corantes isoladamente e em mistura. As concentrações residuais de H2O2 e Fe foram desprezíveis. As mineralizações alcançadas foram da ordem de 50%. Observou-se um aumento de fitotoxicidade após o processo Fenton. Verificou-se, também, o desempenho do processo na presença de dois aditivos comumente usados na indústria têxtil, um igualizante e um anti-espumante. A presença dos aditivos reduziu significativamente os graus de descoramento (de 100% para 90%) e de mineralização (de 50% para 10%). Em relação à fitotoxicidade, verificou-se que os aditivos tornam as soluções muito tóxicas, não tendo sido observado um aumento estatisticamente significativo após o processo Fenton. As análises cromatográficas mostraram, inequivocamente, a presença de pelo menos um produto de oxidação nas amostras tratadas. Concluiu-se que o processo Fenton apresentou um ótimo desempenho para o descoramento dos corantes estudados. Entretanto, a presença dos aditivos tenderia a prejudicar o tratamento de efluentes que contivessem tais corantes. / In the case of industries that use dyeing processes, the removal of color from their wastewaters is a major concern. The azo dyes account for 60% of the dyes currently in use worldwide. However, they are known for their carcinogenic and mutagenic effects, making their treatment an urgent matter. Therefore, several alternatives to the conventional treatment processes have been devised, particularly the Fenton process, which has been proved to be very promising. In this work, the Fenton process optimization regarding the bleaching of two azo dyes was investigated: azorubine (C20H12N2Na2O7S2, C.I. 14720) and tartrazine (C16H7N4Na3O9S2, C.I. 19140). For that purpose, a central composite design was used, a polynomial (empiric) model was fitted to the experimental data, and the optimum conditions were determined: rate [Fe2+]/[H2O2] = 0.64 and 0.32, pH = 1.5 and 2.8, and temperature = 39°C. The response variables were: color removal (measured by the area under the spectrum obtained in the visible region) and the residual concentrations of H2O2 (vanadate method) and Fe (o-fenantroline method). It was determined the mineralization degree by dissolved organic carbon analyses and also the phytotoxicity to lettuce seeds (Lactuca sativa). HPLC-DAD analyses were performed in order to observe the generation of oxidation products. Color removals of approximately 100% were achieved for the each dyes and for a mixture of them. The residual concentrations of H2O2 and Fe were close to zero. Mineralizations around 50% were obtained and a phytotoxicity enhancement after Fenton\'s process. It has also been observed that the performance of that process in the presence of two textile auxiliary products (TAPs) commonly used, a leveling agent and an anti-foaming one. The auxiliaries reduced significantly color removal (from 100% to 90%) and the degree of mineralization (from 50% to 10%). Regarding the phytotoxicity, it was observed that the TAPs used rendered the solutions quite toxic, with no further statistically significant enhancement after the Fenton\'s process. The chromatographic analyses showed, undoubtedly, the presence of at least one oxidation product in the treated samples. It was concluded that the Fenton\'s process presented an excellent performance for removing the color of the studied dyes. However, the presence of the auxiliaries would tend to impair the treatment of wastewaters containing those dyes.

Neste trabalho avaliou-se o comportamento coloidal de suspensões nasais contendo micropartículas de celulose (MCC-NaCMC) com o objetivo de desenvolver um produto genérico compatível com o produto referência de mercado. As propriedades reológicas destas formulações possuem alta influência nos atributos críticos de qualidade do produto, como uniformidade de dose, devido sedimentação durante estocagem em prateleira, e também na performance in-vitro/ in-vivo. Realizaram-se testes com diferentes concentrações de MCC-NaCMC e diferentes parâmetros de processo (tempo e taxa de cisalhamento) utilizando um planejamento de experimentos (DoE) de superfície de respostas através de um modelo composto central. As respostas avaliadas foram tamanho de partículas (quantidade em porcentagem de partículas menores que 1µm e D90) através da técnica por difração a laser e viscosidade/tixotropia através de um reômetro rotacional. Influências significativas dos três fatores e efeitos sinérgicos entre eles nas respostas analisadas foram observadas. Desta maneira foi possível obter respostas próximas ao do produto referência de mercado através deste mapeamento. Observou-se também uma alta correlação entre as respostas, pois este estudo mostrou que o tamanho das partículas coloidais controla a viscosidade e tixotropia das dispersões coloidais. Este trabalho mostrou a significativa influência das etapas de processo no comportamento coloidal das formulações. Idealmente o processo deveria ser monitorado por medidas reológicas, porém este controle é inviável devido ao tempo para a reestruturação do sistema (24 horas). Portanto, a melhor alternativa seria o monitoramento do processo por análise de tamanho de partículas online. / In this work, the colloidal behavior of nasal suspensions containing cellulose microparticles (MCC-NaCMC) was evaluated, in order to develop a generic product compatible with the brand-name product. The rheological properties of these formulations have high influence on the critical quality attributes of the product, such as dose uniformity, due to sedimentation during shelf life, and also on in-vitro/in-vivo performance. Tests were performed with different concentrations of MCC-NaCMC and different process parameters (time and shear rate) using a Design of Experiments (DoE) with response surface by central composite design. The responses evaluated were particle size (amount in percentage of particles smaller than 1m and D90) by means of laser diffraction, and viscosity / thixotropy using a rotational rheometer. Significant influences of the three factors and synergic effects among responses were observed. Through this mapping it was possible to obtain nearby responses to the brand-name product. There was also a strong correlation between the responses, because the size of colloidal particles controlled the dispersion viscosity and thixotropy. This study showed the significant influence of the process steps on the colloidal behavior of the formulations. Ideally the process should be monitored by rheological measurements, but this control is not feasible due to the time required for the system rebuilding (24 hours). Therefore, the best alternative would be monitoring the process by the online particle size analysis.

Hyaluronic acid (HA) is an unbranched polysaccharide consisting of the repeating disaccharide unit β(1→4)-GlcA-β(1→3)-GlcNAc and is a naturally occurring biopolymer in bacteria and vertebras. HA is predominantly found in the extracellular matrix (ECM) and the in vivo function of HA can vary depending on molecular weight (Mw) for instance high Mw HA is reported to be anti-angiogenic while low Mw HA induces angiogenesis. HA is a popular component for hydrogels such as dermal fillers. HA is commonly used in dermal fillers. However, other materials, such as other polymers, can be used as well. The project goal was to investigate different degradation processes for production of target Mw HA. Alkaline and acidic degradation processes in combination with increased temperatures seemed as the most promising methods. Degradation tests performed both in aqueous solution as well as heterogeneously in ethanol were evaluated. The acidic degradation in aqueous solution was proven to have the largest degradation constant. Both a robustness test as well as a Design of Experiments (DoE) was performed to investigate the influence different factors had on the degradation speed. The investigated factors were HA concentration, HCl concentration and temperature. Temperature and HCl concentrations proved to be the most influencing factors and a model was developed in the DoE software MODDE to describe how the factors influenced the degradation constant. The model was established as a good significant model with a Q2 value of 0.998 and relative standard deviation (RSD) value of 0.022 after a logarithmic transformation was performed as well as a simplification of the model by excluding some of the factor interactions. The acidic degradation method also proved to be a highly robust method which easily could be used to produce target Mw HA.

Neste trabalho avaliou-se o comportamento coloidal de suspensões nasais contendo micropartículas de celulose (MCC-NaCMC) com o objetivo de desenvolver um produto genérico compatível com o produto referência de mercado. As propriedades reológicas destas formulações possuem alta influência nos atributos críticos de qualidade do produto, como uniformidade de dose, devido sedimentação durante estocagem em prateleira, e também na performance in-vitro/ in-vivo. Realizaram-se testes com diferentes concentrações de MCC-NaCMC e diferentes parâmetros de processo (tempo e taxa de cisalhamento) utilizando um planejamento de experimentos (DoE) de superfície de respostas através de um modelo composto central. As respostas avaliadas foram tamanho de partículas (quantidade em porcentagem de partículas menores que 1µm e D90) através da técnica por difração a laser e viscosidade/tixotropia através de um reômetro rotacional. Influências significativas dos três fatores e efeitos sinérgicos entre eles nas respostas analisadas foram observadas. Desta maneira foi possível obter respostas próximas ao do produto referência de mercado através deste mapeamento. Observou-se também uma alta correlação entre as respostas, pois este estudo mostrou que o tamanho das partículas coloidais controla a viscosidade e tixotropia das dispersões coloidais. Este trabalho mostrou a significativa influência das etapas de processo no comportamento coloidal das formulações. Idealmente o processo deveria ser monitorado por medidas reológicas, porém este controle é inviável devido ao tempo para a reestruturação do sistema (24 horas). Portanto, a melhor alternativa seria o monitoramento do processo por análise de tamanho de partículas online. / In this work, the colloidal behavior of nasal suspensions containing cellulose microparticles (MCC-NaCMC) was evaluated, in order to develop a generic product compatible with the brand-name product. The rheological properties of these formulations have high influence on the critical quality attributes of the product, such as dose uniformity, due to sedimentation during shelf life, and also on in-vitro/in-vivo performance. Tests were performed with different concentrations of MCC-NaCMC and different process parameters (time and shear rate) using a Design of Experiments (DoE) with response surface by central composite design. The responses evaluated were particle size (amount in percentage of particles smaller than 1m and D90) by means of laser diffraction, and viscosity / thixotropy using a rotational rheometer. Significant influences of the three factors and synergic effects among responses were observed. Through this mapping it was possible to obtain nearby responses to the brand-name product. There was also a strong correlation between the responses, because the size of colloidal particles controlled the dispersion viscosity and thixotropy. This study showed the significant influence of the process steps on the colloidal behavior of the formulations. Ideally the process should be monitored by rheological measurements, but this control is not feasible due to the time required for the system rebuilding (24 hours). Therefore, the best alternative would be monitoring the process by the online particle size analysis.

Orientador: Messias Borges Silva / Resumo: O cultivo de microalgas tem sido considerado como uma fonte promissora de lipídeos para a obtenção de ácidos graxos de alto valor agregado, como é o caso dos ômegas 3 (ω3) e ômegas 6 (ω6). O uso do planejamento de experimentos (DOE) permite estabelecer condições apropriadas de cultivo para as microalgas que favorece o acúmulo desses ácidos graxos. Desta forma, o presente trabalho teve como objetivo melhorar o desempenho dos cultivos das microalgas Nannochloropsis gaditana e Dunaliella salina, visando a produção de ω3 e ω6. Primeiramente, foram avaliadas, com o uso de uma matriz ortogonal Taguchi L4, as influências das concentrações de nitrato de sódio (de 25 a 75 mg L-1), de acetato de sódio e bicarbonato de sódio (ambas de 0 a 2 g L-1), sobre a produtividade de biomassa (Pb) e de lipídeos (Po). Como resultado, foi notado que tanto o acetato quanto o nitrato, influenciaram positivamente na Pb e na Po, para ambas as microalgas estudadas. O bicarbonato, por outro lado, não melhorou a Po, sendo excluído das etapas posteriores. Na etapa seguinte do trabalho foi realizado um planejamento fatorial completo 22 com ponto central, focando no estudo da concentração de nitrato (75 a 225 mg L-1) e acetato (2 a 6 gL-1) sobre a produtividade dos cultivos. As maiores Pb obtidas foram: 188,93 mg L-1 dia-1 para a microalga N. gaditana (225 mg L-1 de nitrato e 6 g L-1 de acetato) e 118,93 mg L-1 dia-1 para a D. salina (150 mg L-1 de nitrato e 4 g L-1 de acetato). Nestas condições de cultivo, a... (Resumo completo, clicar acesso eletrônico abaixo) / Doutor