Thesis (M.S.)--University of Nevada, Reno, 2007. / "May, 2007." Includes bibliographical references. Online version available on the World Wide Web.

Thesis (M.S.)--University of Tennessee, Knoxville, 2009. / Title from title page screen (viewed on Oct. 23, 2009). Thesis advisor: David K. Irick. Vita. Includes bibliographical references.

Thesis (M.S.)--West Virginia University, 2006. / Title from document title page. Document formatted into pages; contains ix, 89 p. : ill. (some col.). Includes abstract. Includes bibliographical references (p. 67-70).

Thesis (M.S.)--West Virginia University, 2007. / Title from document title page. Document formatted into pages; contains xiii, 145 p. : ill. (some col.). Includes abstract. Includes bibliographical references (p. 84-87).

A qualidade dos combustíveis é um dos principais fatores que afetam o desempenho dos motores de combustão interna e é caracterizada por um conjunto de propriedades físicas e químicas. Neste trabalho foi investigada a influência da temperatura sobre algumas propriedades como a densidade, viscosidade dinâmica, ponto de névoa e de fluidez de diferentes combustíveis. Além disso, medidas envolvendo termogravimetria e espectrometria na região do infravermelho médio também foram conduzidas. Medidas de densidade em função da temperatura ou da concentração de biodiesel na amostra revelaram uma dependência linear, de forma que a redução da temperatura ou o aumento da concentração de biodiesel provocaram um aumento da densidade. O estudo reológico a partir de medidas de viscosidade permitiu identificar o comportamento de fluido Newtoniano para todas as amostras analisadas. Um ajuste exponencial do tipo Arrhenius foi utilizado para analisar a correlação entre viscosidade dinâmica e temperatura, possibilitando identificar uma temperatura limite, T*, abaixo da qual esse ajuste não é mais satisfeito e o processo de solidificação da amostra é desencadeado. Um diagrama de fases em função das temperaturas T*, do ponto de névoa e de fluidez foi elaborado, possibilitando identificar, em função da concentração de biodiesel da amostra, faixas de temperaturas onde as fases líquidas e/ou sólidas podem ser encontradas, bem como onde o ajuste entre a viscosidade dinâmica e a temperatura pode ser obtido por uma equação exponencial do tipo Arrhenius. Além disso, medidas calorimétricas revelaram uma maior energia por unidade de massa para as amostras de diesel padrão, e que esta energia decresce linearmente com o incremento da concentração de biodiesel na amostra. Termogramas revelaram diferentes perfis de degradação térmica para as amostras, de forma que um deslocamento da curva de degradação para temperaturas mais elevadas foi observado em função do aumento do teor de enxofre nas amostras de diesel padrão assim como pelo incremento da concentração de biodiesel nas amostras produzidas pela mistura entre diesel e biodiesel. A análise das amostras líquidas utilizando radiação com comprimento de ondas no infravermelho permitiram identificar diferentes grupos funcionais presentes nas amostras e estabelecer, em termos da intensidade da absorbância característica da dupla ligação Carbono-Oxigênio presentes nos ésteres do biodiesel, uma relação com a concentração de biodiesel presente na amostra. Neste sentido, por meio da análise de diferentes propriedades físicas e químicas das amostras estudadas, foi possível avaliar características e interdependências destas propriedades, principalmente no que diz respeito a variações da temperatura. Sendo assim, ao longo deste trabalho, são apresentados dados e apontamentos importantes para tratar do tema abordado. / Fuel quality is a major factor affecting the performance of internal combustion engines and it is characterized by a combination of physical and chemical properties. In this study, the influence of temperature on some properties such as density, dynamic viscosity, cloud point and pour point were investigated in different samples of fuels. In addition, measurements involving thermogravimetry and infrared spectroscopy were also performed. Density measurements as a function of temperature or concentration of biodiesel in the sample revealed a linear dependence, indicating that the temperature reduction or increase of the concentration of biodiesel results in a density increase. The rheological study from dynamic viscosity measurements identified the Newtonian fluid behavior for all samples. It was also observed an increase in the dynamic viscosity caused by the increase of the concentration of biodiesel in the sample and also the reducing the temperature. An exponential fit of the Arrhenius type equation was used to analyze the correlation between dynamic viscosity and temperature, allowing to identify a temperature limit, T*, below which this adjustment is lost and the sample solidification process is triggered. A phase diagram as a function of the biodiesel concentration and the temperature T*, the cloud point and poor point was prepared. This diagram shows the temperature ranges in which liquid and/or solid phases can be found, and where the fit between the temperature and dynamic viscosity can be obtained by an exponential equation of Arrhenius type. In addition, calorimetric measurements revealed a higher energy per mass unit for the standard diesel samples, and that this energy decreases linearly with increasing of biodiesel content. Thermal analysis showed different degradation profiles for the samples. Thermograms indicated a shift of the degradation curve at higher temperatures due to the increase in the sulfur content in the samples of standard diesel and also increasing the biodiesel concentration in the samples produced by mixture of diesel and biodiesel. The analysis of liquid samples using infrared radiation allowed the identification of different functional groups present in the samples and to establish, in terms of the intensity of the absorbance characteristic of the carbon-oxygen double bond present in the esters of biodiesel, a relation with the concentration of biodiesel present in the sample. In this sense, through the analysis of different physical and chemical properties of the samples, it was possible to evaluate characteristics and interrelationships of these properties, particularly in respect of temperature variations, which can favor or disfavor the increased biodiesel concentration in blends with diesel. Thus, throughout this study are presented important data and notes related with the theme.

A qualidade dos combustíveis é um dos principais fatores que afetam o desempenho dos motores de combustão interna e é caracterizada por um conjunto de propriedades físicas e químicas. Neste trabalho foi investigada a influência da temperatura sobre algumas propriedades como a densidade, viscosidade dinâmica, ponto de névoa e de fluidez de diferentes combustíveis. Além disso, medidas envolvendo termogravimetria e espectrometria na região do infravermelho médio também foram conduzidas. Medidas de densidade em função da temperatura ou da concentração de biodiesel na amostra revelaram uma dependência linear, de forma que a redução da temperatura ou o aumento da concentração de biodiesel provocaram um aumento da densidade. O estudo reológico a partir de medidas de viscosidade permitiu identificar o comportamento de fluido Newtoniano para todas as amostras analisadas. Um ajuste exponencial do tipo Arrhenius foi utilizado para analisar a correlação entre viscosidade dinâmica e temperatura, possibilitando identificar uma temperatura limite, T*, abaixo da qual esse ajuste não é mais satisfeito e o processo de solidificação da amostra é desencadeado. Um diagrama de fases em função das temperaturas T*, do ponto de névoa e de fluidez foi elaborado, possibilitando identificar, em função da concentração de biodiesel da amostra, faixas de temperaturas onde as fases líquidas e/ou sólidas podem ser encontradas, bem como onde o ajuste entre a viscosidade dinâmica e a temperatura pode ser obtido por uma equação exponencial do tipo Arrhenius. Além disso, medidas calorimétricas revelaram uma maior energia por unidade de massa para as amostras de diesel padrão, e que esta energia decresce linearmente com o incremento da concentração de biodiesel na amostra. Termogramas revelaram diferentes perfis de degradação térmica para as amostras, de forma que um deslocamento da curva de degradação para temperaturas mais elevadas foi observado em função do aumento do teor de enxofre nas amostras de diesel padrão assim como pelo incremento da concentração de biodiesel nas amostras produzidas pela mistura entre diesel e biodiesel. A análise das amostras líquidas utilizando radiação com comprimento de ondas no infravermelho permitiram identificar diferentes grupos funcionais presentes nas amostras e estabelecer, em termos da intensidade da absorbância característica da dupla ligação Carbono-Oxigênio presentes nos ésteres do biodiesel, uma relação com a concentração de biodiesel presente na amostra. Neste sentido, por meio da análise de diferentes propriedades físicas e químicas das amostras estudadas, foi possível avaliar características e interdependências destas propriedades, principalmente no que diz respeito a variações da temperatura. Sendo assim, ao longo deste trabalho, são apresentados dados e apontamentos importantes para tratar do tema abordado. / Fuel quality is a major factor affecting the performance of internal combustion engines and it is characterized by a combination of physical and chemical properties. In this study, the influence of temperature on some properties such as density, dynamic viscosity, cloud point and pour point were investigated in different samples of fuels. In addition, measurements involving thermogravimetry and infrared spectroscopy were also performed. Density measurements as a function of temperature or concentration of biodiesel in the sample revealed a linear dependence, indicating that the temperature reduction or increase of the concentration of biodiesel results in a density increase. The rheological study from dynamic viscosity measurements identified the Newtonian fluid behavior for all samples. It was also observed an increase in the dynamic viscosity caused by the increase of the concentration of biodiesel in the sample and also the reducing the temperature. An exponential fit of the Arrhenius type equation was used to analyze the correlation between dynamic viscosity and temperature, allowing to identify a temperature limit, T*, below which this adjustment is lost and the sample solidification process is triggered. A phase diagram as a function of the biodiesel concentration and the temperature T*, the cloud point and poor point was prepared. This diagram shows the temperature ranges in which liquid and/or solid phases can be found, and where the fit between the temperature and dynamic viscosity can be obtained by an exponential equation of Arrhenius type. In addition, calorimetric measurements revealed a higher energy per mass unit for the standard diesel samples, and that this energy decreases linearly with increasing of biodiesel content. Thermal analysis showed different degradation profiles for the samples. Thermograms indicated a shift of the degradation curve at higher temperatures due to the increase in the sulfur content in the samples of standard diesel and also increasing the biodiesel concentration in the samples produced by mixture of diesel and biodiesel. The analysis of liquid samples using infrared radiation allowed the identification of different functional groups present in the samples and to establish, in terms of the intensity of the absorbance characteristic of the carbon-oxygen double bond present in the esters of biodiesel, a relation with the concentration of biodiesel present in the sample. In this sense, through the analysis of different physical and chemical properties of the samples, it was possible to evaluate characteristics and interrelationships of these properties, particularly in respect of temperature variations, which can favor or disfavor the increased biodiesel concentration in blends with diesel. Thus, throughout this study are presented important data and notes related with the theme.

M.Tech. (Chemical Engineering) / Please refer to full text to view abstract

Typescript (photocopy). / Digitized by Kansas Correctional Industries

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Solid basic metal oxides have been extensively studied for biodiesel production via transesterification, researches are now focused on attaining high catalytic activity and durability towards one-step alkali transesterification, as well as high stability towards high free fatty acids (FFAs) and water content in oils for simultaneous esterification and transesterification, to enable their commercialization in industry. This work encompasses the design and characterization of three mixed metal oxide systems, with a detailed evaluation of their potential application in catalyzing transesterification of camelina oil to yield biodiesel. Na0.1Ca0.9TiO3 nanorods were synthesized via a simple alkaline hydrothermal pathway with ethanol as a co-solvent. Owing to their high basic strength of 11<H_<15, 92.7% biodiesel conversion was reached at mild reaction conditions. However, the catalyst showed poor recycle performance, probably attributed to the leaching of active species during transesterification, as revealed by X-ray photoelectron spectroscopy (XPS). A new class of mesoporous Zn/MgO catalyst was synthesized by a simple alkaline hydrothermal method. Zn/MgO calcinated at 600 ℃ exhibited 88.7% biodiesel conversion at 120 ℃ with 3% w/w catalyst, 24:1 methanol to oil molar ratio for 8 h. The catalyst could be reused for five runs without significant loss of activity (≥84.0% biodiesel conversion). The excellent catalyst performance is possibly attributed to its high surface area and large mesopores. The higher surface basic sites density as compared to mesoporous MgO, as indicated by higher total basicity determined from benzoic titration and an increased lattice O2- percentage as revealed from XPS, attributing to its superior catalytic activity. A series of nano-sized MgO-ZnO catalysts with precise stoichiometry were successfully prepared by a simple EDTA complexing approach. Mg0.5Zn0.5 calcinated at 600 ℃ gave a maximum biodiesel conversion of 89.3% at 120 ℃ with 3% w/w catalyst, 24:1 methanol to oil molar ratio for 8 h. Its superior catalytic performance to MgO is mainly associated with the high basic sites density as determined from benzoic titration and XPS. The biodiesel conversion retained over 83.0% for five runs. The enhanced catalyst activity and stability might be contributed by the incorporation of Zn2+ for Mg2+ in MgO lattice and a high homogeneous distribution of MgO particles on ZnO, with the formation of Mg-O-Zn bond as evidenced by Fourier transform infrared spectroscope (FTIR) and XPS. The catalyst also demonstrated high tolerance to FFAs (10% w/w) and water (2% w/w) content, which make it desirable for direct conversion of oils with high FFAs level to biodiesel in a single-step process. Lastly, a Zn/La2O3 catalyst was synthesized by a simple hydrothermal pathway. It exhibits a higher basic strength than La2O3, as evidenced by the slightly lower O1s binding energy determined by XPS, leading to a higher catalytic activity. The enhanced catalytic activity and stability is likely contributed by the incorporation of Zn2+ for La3+ in the lattice. Using 1% w/w Zn/La2O3 as catalyst, the highest biodiesel conversion of 92.7% was obtained at 120 ℃ for 16 h with 36:1 methanol to oil molar ratio. The effective catalyst displayed a biodiesel conversion greater than 84.0% for four runs. / published_or_final_version / Chemistry / Doctoral / Doctor of Philosophy