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Biofuels are becoming more attractive worldwide because of the high energy demands and the fossil fuel resources that are being depleted. Biodiesel is one of the most attractive alternative energy sources to petroleum diesel fuel and it is renewable, non toxic, biodegradable, has low sulphur content and has a high flash point. Biodiesel can be generated from domestic natural resources such as coconuts, rapeseeds, soybeans, sunflower, and waste cooking oil through a commonly used method called transesterification. Transesterification is a reaction whereby oil (e.g. sunflower oil) or fats react with alcohol (e.g. methanol) with or without the presence of a catalyst (e.g. potassium hydroxide) to form fatty acid alkyl esters (biodiesel) and glycerol. The high-energy input for biodiesel production remains a concern for the competitive production of bio-based transportation fuels. However, microwave radiation is a method that can be used in the production of biodiesel to reduce the reaction time as well as to improve product yields. Sunflower oil is one of the biodiesel feedstocks that are used in South Africa and is widely used in cooking and for frying purposes. This study aims to use microwave irradiation to reduce the energy input for biodiesel production. The effect of various reaction variables, including reaction time (10 – 60 seconds), microwave power (300 – 900 watts), catalyst (potassium hydroxide) loading (0.5 – 1.5 wt%) and methanol to oil molar ratio (1:3 – 1:9) on the yield of fatty acid methyl ester (biodiesel) was investigated. The quality of biodiesel produced was analysed by Gas Chromatography (GC), Fourier Transform Infrared Spectroscopy (FTIR) and viscometry. The FTIR results confirmed the presence of functional groups of the FAME produced during transesterification. The results showed that transesterification can proceed much faster under microwave irradiation than when using traditional heating methods. The interaction between the alcohol and oil molecules is significantly improved, leading to shorter reaction times (seconds instead of hours) and improved diesel yields. The highest biodiesel yield obtained was 98% at 1:6 oil-to-methanol molar ratio for both 1 wt% and 1.5 wt% potassium hydroxide (KOH) at a reduced reaction time (30 seconds). The chemical composition of FAME (biodiesel) obtained from different conditions i contained palmitic acid (C16:0), stearic acid (C18:0), oleic acid (C18:1) and 70% linoleic acid (C18:2). The physical properties (cetane number, viscosity, density and FAME content) of biodiesel produced met the SANS 1935 specification. The energy consumption was reduced from 1.2 kWh with the traditional transesterification to 0.0067 kWh with the microwave transesterification. Microwave irradiation was shown to be effective in significantly lowering the energy consumption for production of biodiesel with good quality for small scale producers. / Thesis (MSc (Engineering Sciences in Chemical Engineering))--North-West University, Potchefstroom Campus, 2013

Biofuels are becoming more attractive worldwide because of the high energy demands and the fossil fuel resources that are being depleted. Biodiesel is one of the most attractive alternative energy sources to petroleum diesel fuel and it is renewable, non toxic, biodegradable, has low sulphur content and has a high flash point. Biodiesel can be generated from domestic natural resources such as coconuts, rapeseeds, soybeans, sunflower, and waste cooking oil through a commonly used method called transesterification. Transesterification is a reaction whereby oil (e.g. sunflower oil) or fats react with alcohol (e.g. methanol) with or without the presence of a catalyst (e.g. potassium hydroxide) to form fatty acid alkyl esters (biodiesel) and glycerol. The high-energy input for biodiesel production remains a concern for the competitive production of bio-based transportation fuels. However, microwave radiation is a method that can be used in the production of biodiesel to reduce the reaction time as well as to improve product yields. Sunflower oil is one of the biodiesel feedstocks that are used in South Africa and is widely used in cooking and for frying purposes. This study aims to use microwave irradiation to reduce the energy input for biodiesel production. The effect of various reaction variables, including reaction time (10 – 60 seconds), microwave power (300 – 900 watts), catalyst (potassium hydroxide) loading (0.5 – 1.5 wt%) and methanol to oil molar ratio (1:3 – 1:9) on the yield of fatty acid methyl ester (biodiesel) was investigated. The quality of biodiesel produced was analysed by Gas Chromatography (GC), Fourier Transform Infrared Spectroscopy (FTIR) and viscometry. The FTIR results confirmed the presence of functional groups of the FAME produced during transesterification. The results showed that transesterification can proceed much faster under microwave irradiation than when using traditional heating methods. The interaction between the alcohol and oil molecules is significantly improved, leading to shorter reaction times (seconds instead of hours) and improved diesel yields. The highest biodiesel yield obtained was 98% at 1:6 oil-to-methanol molar ratio for both 1 wt% and 1.5 wt% potassium hydroxide (KOH) at a reduced reaction time (30 seconds). The chemical composition of FAME (biodiesel) obtained from different conditions i contained palmitic acid (C16:0), stearic acid (C18:0), oleic acid (C18:1) and 70% linoleic acid (C18:2). The physical properties (cetane number, viscosity, density and FAME content) of biodiesel produced met the SANS 1935 specification. The energy consumption was reduced from 1.2 kWh with the traditional transesterification to 0.0067 kWh with the microwave transesterification. Microwave irradiation was shown to be effective in significantly lowering the energy consumption for production of biodiesel with good quality for small scale producers. / Thesis (MSc (Engineering Sciences in Chemical Engineering))--North-West University, Potchefstroom Campus, 2013

This diploma thesis provides summary information about using of near infrared spectroscopy for monitoring of high oleic acid content in sunflower seed. The calibration for high oleic sunflower seed was performed by using calibration model PLS - „Partial least squares. Gas chromatography was used as a reference method. Based on this knowledge thirty samples of high oleic sunflower seeds were measured and evaluated on this calibration. The last part of diploma thesis consist of comparison of oleic acid results measured by near infrared spectroscopy and gas chromatography used as reference method, and discussion about the measurement accuracy and evaluation of suitability of using these methods.

Durante anos, a manteiga foi muito apreciada pelo consumidor, mas por conter grande quantidade de ácidos graxos saturados e colesterol, seu consumo tem diminuído. Recentemente, a descoberta dos malefícios causados pelos ácidos graxos trans presentes nas margarinas produzidas por hidrogenação parcial aumentou o interesse por métodos alternativos de modificação de lipídios. Assim, o objetivo deste trabalho foi desenvolver um lipídio estruturado à base de gordura do leite que apresentasse maiores teores de ácidos graxos insaturados que a manteiga original e, consequentemente, melhor espalhabilidade, além de conter fitosteróis, constituindo a base de um alimento funcional com capacidade de reduzir os níveis de colesterol no sangue. Foram realizadas misturas da gordura do leite (GL) com óleo de girassol (OG) e ésteres de fitosteróis (EF) e foi efetuada interesterificação química e enzimática. As misturas e os lipídios estruturados obtidos foram analisados quanto a composição em ácidos graxos, consistência, conteúdo de gordura sólida (CGS), cinética de cristalização e estrutura cristalina, entre outras propriedades físico-químicas. Foram obtidos produtos contendo cerca de 60% de ácidos graxos insaturados pela adição de até 40% de OG e 25% de EF à gordura do leite, que originalmente possuía cerca de 33% de ácidos graxos insaturados. A interesterificação química melhorou a plasticidade das misturas, enquanto que a modificação enzimática não modificou de maneira expressiva sua consistência. A adição de pequenas quantidades de OG à GL provocou grande diminuição de sua consistência, enquanto que a diminuição do CGS ocorreu em proporções semelhantes às esperadas por interpolação linear. A edição de vídeos que permitam a observação da formação da estrutura cristalina de gorduras mostrou ser uma ferramenta de grande utilidade no estudo da cristalização de óleos e gorduras. A emulsão preparada com a mistura contendo 25,0% de EF, 7,5% de OG e 67,5% de GL apresentou diminuição expressiva na consistência quando comparada à manteiga, representando um efeito benéfico. / For many years, butter has been held in the highest esteem by consumer but its world consumption has steadily declined due to its high contents of saturated fatty acids and cholesterol. More recently, trans fatty acids, which are commonly resent in hydrogenated argarines, have been found to cause detrimental effects when consumed in high amounts. This observation has increased the interest in alternative methods of lipid modification. Therefore, the objective of this work was to develop a milkfat based structured lipid, presenting higher contents of unsaturated fatty acids than original butter and consequently better spreadability, besides containing phytosterols and serving as a base of a functional food with a cholesterol lowering health claim. Blends containing milkfat (MF), sunflower oil (SO) and phytosterol esters (PE) were prepared and then chemically and enzimatically interesterified. The fatty acid composition, consistency, solid fat content (SFC), crystallization kinetics and crystal structure, among other physical and chemical properties were analyzed. The blends presented about 60% of unsaturated fatty acids with the addition of up to 40% of SO and 25% of PE to MF, which originally presented close to 33% of unsaturated fatty acids. Chemical interesterification improved the plasticity of the blends, while the enzymatic reaction did not substantially alter it. The addition of small amounts of SO and PE to MF caused a great decrease in its consistency, while SFC decreased almost proportionally to the addition of these components. The edition of videos made possible the observation of crystal structure formation and it represented a tool of great importance in the fats and oils crystallization research. The emulsion prepared with the blend containing 25.0% of PE, 7.5% of SO, and 67.5% of MF presented a substantial improvement in consistency when compared to butter commercially available.

Durante anos, a manteiga foi muito apreciada pelo consumidor, mas por conter grande quantidade de ácidos graxos saturados e colesterol, seu consumo tem diminuído. Recentemente, a descoberta dos malefícios causados pelos ácidos graxos trans presentes nas margarinas produzidas por hidrogenação parcial aumentou o interesse por métodos alternativos de modificação de lipídios. Assim, o objetivo deste trabalho foi desenvolver um lipídio estruturado à base de gordura do leite que apresentasse maiores teores de ácidos graxos insaturados que a manteiga original e, consequentemente, melhor espalhabilidade, além de conter fitosteróis, constituindo a base de um alimento funcional com capacidade de reduzir os níveis de colesterol no sangue. Foram realizadas misturas da gordura do leite (GL) com óleo de girassol (OG) e ésteres de fitosteróis (EF) e foi efetuada interesterificação química e enzimática. As misturas e os lipídios estruturados obtidos foram analisados quanto a composição em ácidos graxos, consistência, conteúdo de gordura sólida (CGS), cinética de cristalização e estrutura cristalina, entre outras propriedades físico-químicas. Foram obtidos produtos contendo cerca de 60% de ácidos graxos insaturados pela adição de até 40% de OG e 25% de EF à gordura do leite, que originalmente possuía cerca de 33% de ácidos graxos insaturados. A interesterificação química melhorou a plasticidade das misturas, enquanto que a modificação enzimática não modificou de maneira expressiva sua consistência. A adição de pequenas quantidades de OG à GL provocou grande diminuição de sua consistência, enquanto que a diminuição do CGS ocorreu em proporções semelhantes às esperadas por interpolação linear. A edição de vídeos que permitam a observação da formação da estrutura cristalina de gorduras mostrou ser uma ferramenta de grande utilidade no estudo da cristalização de óleos e gorduras. A emulsão preparada com a mistura contendo 25,0% de EF, 7,5% de OG e 67,5% de GL apresentou diminuição expressiva na consistência quando comparada à manteiga, representando um efeito benéfico. / For many years, butter has been held in the highest esteem by consumer but its world consumption has steadily declined due to its high contents of saturated fatty acids and cholesterol. More recently, trans fatty acids, which are commonly resent in hydrogenated argarines, have been found to cause detrimental effects when consumed in high amounts. This observation has increased the interest in alternative methods of lipid modification. Therefore, the objective of this work was to develop a milkfat based structured lipid, presenting higher contents of unsaturated fatty acids than original butter and consequently better spreadability, besides containing phytosterols and serving as a base of a functional food with a cholesterol lowering health claim. Blends containing milkfat (MF), sunflower oil (SO) and phytosterol esters (PE) were prepared and then chemically and enzimatically interesterified. The fatty acid composition, consistency, solid fat content (SFC), crystallization kinetics and crystal structure, among other physical and chemical properties were analyzed. The blends presented about 60% of unsaturated fatty acids with the addition of up to 40% of SO and 25% of PE to MF, which originally presented close to 33% of unsaturated fatty acids. Chemical interesterification improved the plasticity of the blends, while the enzymatic reaction did not substantially alter it. The addition of small amounts of SO and PE to MF caused a great decrease in its consistency, while SFC decreased almost proportionally to the addition of these components. The edition of videos made possible the observation of crystal structure formation and it represented a tool of great importance in the fats and oils crystallization research. The emulsion prepared with the blend containing 25.0% of PE, 7.5% of SO, and 67.5% of MF presented a substantial improvement in consistency when compared to butter commercially available.

Mechanical pressing of soybean is highly desirable as it provides, at low cost, non-contaminated, protein-rich, low-fat soyflour which can be further processed into nutritious edible foods. Unfortunately, mechanical pressing of this low-fat oilseed ($<$20%) yields only 50-70% of the available oil, in contrast to the solvent extraction method which recovers over 98% of the oil. The main focus of the study was to maximize the oil recovery from soybean using mechanical oil expression by applying two pretreatments, enzymatic hydrolysis and extrusion cooking of soybeans, and by varying the pressing conditions including three applied pressures (20, 40 and 60 MPa), three pressing temperatures (22, 60 and 90°C) and two sample sizes (10 and 20 g). To characterize the material properties affecting mechanical oil expression from soybean a mathematical simulation of uniaxial compression was developed which incorporated the time dependent variation of soybean properties. The mathematical simulation was based on Terznaghi's theory of consolidation for soils and was solved using measured values of the coefficients of permeability, volume change and consolidation. A compression-permeability test cell was specifically developed for these measurements. For validation of the model, in addition to extruded soy, sunflower seeds (oil content ca. 45%) were also compressed under the same pressing conditions. Improvements in oil recovery due to enzymatic pretreatment of soybean were small, while the extrusion pretreatment increased the oil recovery from only a trace for raw soybean to 90.6%. Such oil recovery using mechanical pressing of soybean has not been reported in the past. The measured values of oil recovery, coefficients of permeability, volume change and consolidation for soybean and sunflower seeds were found to vary significantly $(P<0.05)$ with time of pressing, applied pressure, pressing temperature and the size of the sample. For extruded soy samples, the developed model predicted the values of oil recovery versus pressing time with an average error of 15%, while for sunflower seed samples the average prediction error was 40%. The high error values were attributed to the presence of hulls in the sunflower seed samples, as well as error during measurement of the coefficient of permeability. The coefficient of consolidation was found to have the greatest influence on oil recovery. The incorporation of time dependent material properties in the developed simulation was demonstrated to give more accurate and consistent prediction in trends of oil recovery as compared to using constant material properties. The correlationship developed between the oilseed material properties and the oil recovery obtained from uniaxially compressed oilseeds would help researchers and designers to better evaluate the mechanical oil expression equipment and systems. To the extent that the developed model adequately predicted oil recoveries from both sunflower and soybean oilseeds, the model is expected to be applicable to other oilseeds as well.

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