Thesis (Diploma)--University of the Witwatersrand.

Thesis (Ph.D.)--Virginia Commonwealth University, 2008. / Title from title-page of electronic thesis. Prepared for: Dept. of Mechanical Engineering. Bibliography: leaves 212-233.

Thesis (Ph. D.)--Virginia Commonwealth University, 2008. / Prepared for: Dept. of Mechanical Engineering. Includes bibliographical references (leaves 212-233). Also available online via the Internet.

The research carried out in this thesis describes the processing of liquids and ceramic suspensions, having a viscosity >100mPa s, using electrostatic atomization, mainly in the stable cone-jet mode. Electrostatic atomization, also called electrospraying, refers to a process where a liquid or a suspension is made to flow through a needle. The liquid or suspension is subjected to a high voltage maintained between the needle and a ground electrode. Two major physical properties, namely electrical conductivity and viscosity, affect electrostatic atornization in the stable cone-jet mode and the investigations described in this thesis focussed on the latter. Firstly, a set of liquid mixtures were prepared using distilled water and glycerol. The dc electrical conductivity of these mixtures were kept constant and the viscosity was varied. The mixtures were subjected to electrostatic atornization and in each case the mode of atornization, the cone/jet characteristics and relic sizes were studied as a function of viscosity. The effect of applied voltage on the conejet mode electrostatic atornization of glycerol having a viscosity of 1338mPa s was also investigated. Secondly, the possibilities of electrostatically atomizing ceramic suspensions were studied in detail. Several alumina suspensions were used including one containing a high volume fraction of solids (20 vol. % - the highest filler loading attempted to date using any jet-based processing route). Applied voltage - flow rate - atornization mode maps were constructed for this suspension incorporating even pico-flow rate regimes. This is a new input into the aerosol science and engineering literature. This section also highlights the importance of controlling the applied voltage and flow rate as these parameters affect the jet diameter and relic/droplet size generated. The effect of the geometry of the ground electrode used for electrostatic atornization was also investigated. In particular, the use of a point-like ground electrode was studied for the very first time. The third and most innovative facet of this research was the discovery of ceramic electrostatic atornization printing (CEAP) and the use of electrostatic atornization to produce ceramic foams. In CEAP a point-like ground electrode is used to focus the spray which was printed as characters, collection of characters and single tracks. This investigation was extended to explore the printing of multiple tracks produced with the aid of several needles and ground electrodes which worked simultaneously. A ring shaped ground electrode was used to electrospray ceramic droplets onto a polyurethane template and this paved the way for the development of a new method to prepare open-cell ceramic foams with a very high porosity. This method was extended to prepare ceramic structures and complex components.

Kin-Fai Ho. / Thesis (M.Phil.)--Chinese University of Hong Kong, 1999. / Includes bibliographical references (leaves [61-66]). / Abstracts in English and Chinese. / Contents / ACKNOWLEDGMENT / ABSTRACT / Chapter CHAPTER 1 --- INTRODUCTION / Chapter 1.1 --- Air Pollution in Hong Kong / Chapter 1.2 --- Brief introduction of Particulate Matter / Chapter 1.2.1 --- Total suspended particulates / Chapter 1.2.2 --- Respirable suspended particulates / Chapter 1.2.3 --- PM2.5 / Chapter 1.3 --- Lead in Air Particulate and its Harmful Effects on Human / Chapter 1.4 --- Air Sampling / Chapter 1.5 --- Sample Treatment / Chapter 1.5.1 --- Acid digestion method / Chapter 1.5.2 --- Slurry sampling method / Chapter 1.5.3 --- Comparison between acid digestion and slurry sampling method / Chapter 1.5.4 --- Chemical modification / Chapter CHAPTER 2 --- EXPERIMENTAL / Chapter 2.1 --- Apparatus / Chapter 2.2 --- Instrumental analysis / Chapter 2.2.1 --- Electrothermal atomic absorption spectrometry / Chapter 2.2.2 --- Background correction by the Zeeman effect / Chapter 2.3 --- Reagents / Chapter 2.4 --- Procedure / Chapter 2.4.1 --- Collection of air sample / Chapter 2.4.2 --- Treatment of sample collected on filter / Chapter 2.4.2.1 --- Digestion Procedure / Chapter 2.4.2.2 --- Procedure for Slurry Preparation / Chapter 2.4.3 --- Temperature program employed / Chapter 2.4.4 --- Sample introduction / Chapter 2.4.5 --- Determination of Lead in PM 2.5 by Acid Digestion Method / Chapter 2.4.6 --- Determination of Lead in PM 2.5 by Developed Method / Chapter 2.4.7 --- Study of particle size and suspension behavior of PM 2.5 in solvent / Chapter CHAPTER 3 --- RESULTS AND DISCUSSION / Chapter 3.1 --- Choice of filter for air sampling / Chapter 3.2 --- Choice of Solvents for Suspension of Air Particulates / Chapter 3.3 --- Ultrasonic agitation / Chapter 3.4 --- Effect of the sonication time / Chapter 3.5 --- Particle size and Effect of stabilization agents / Chapter 3.6 --- Effect of acid predigestion of the slurry sample / Chapter 3.7 --- Chemical Modification / Chapter 3.7.1 --- Use palladium as chemical modifier / Chapter 3.7.2 --- Amount of chemical modifier / Chapter 3.7.3 --- Effect of nitric acid / Chapter 3.8 --- Optimization of the graphite furnace temperature / Chapter 3.9 --- Effect of using platform / Chapter 3.10 --- Sample injection volume / Chapter 3.11 --- Recovery study of Lead in PM2.5 / Chapter 3.12 --- The limit of detection and precision of the developed method / Chapter CHAPTER 4 --- CONCLUSION / APPENDIX / REFERENCES

O eugenol é um composto fenólico natural que apresenta atividade antioxidante e antimicrobiana e o seu uso como substituto de aditivos sintéticos em alimentos tem sido proposto. Contudo, pela sua instabilidade frente aos agentes externos (luz, oxigênio e calor), seu uso no processamento de alimentos é comprometido. Assim, a microencapsulação é uma alternativa viável para sua aplicação. Os objetivos deste trabalho foram avaliar o efeito da variação das condições operacionais do atomizador (temperatura do ar de entrada e vazão de alimentação) na obtenção de eugenol microencapsulado em carragena, e estudar a influência da combinação de carragena e proteína do farelo de arroz, albumina sérica bovina e proteína do soro de leite com baixo teor de lactose na microencapsulação de eugenol. Em uma primeira etapa, um Delineamento Composto Central Rotacional (DCCR) do tipo 22 com duas variáveis independentes (temperatura do ar de secagem e vazão de alimentação), três pontos centrais e quatro pontos axiais, foi desenvolvido para avaliar as condições operacionais de atomização. A quantificação do eugenol, recuperação (RE %) e a eficiência de encapsulação (EE %) foi avaliadada por espectrofometria UV-Vis e a morfologia por microscopia ótica. Na segunda etapa, a influência do uso de carragena em combinação com proteína do farelo de arroz, albumina sérica bovina e proteína do soro de leite com baixo teor de lactose foi avaliada por meio de um planejamento de mistura do tipo simplex-centroid. A caracterização das microcápsulas foi determinada pela RE % e EE % por Cromatografia Líquida de Alta Eficiência (CLAE), análise termogravimétrica acoplada à espectrofotometria de infravermelho e, morfologia por microscopia eletrônica de varredura. Para o DCCR, o valor máximo de RE% obtido foi de 12% e as condições operacionais estudadas não influenciaram significativamente (p > 0,05). Já a EE% variou de 18,0 a 84,8% e, o termo quadrático para vazão de alimentação apresentou influência significativa (p ≤ 0,05) na resposta avaliada. Para o planejamento simplex-centroid, o valor médio de RE % das microcápsulas variou de 37,9 a 104,5% e o de EE% de 0,0 a 79,4%, sendo que ambas as respostas foram influenciadas (p ≤ 0,05%) pelos agentes encapsulantes da formulação. A albumina sérica bovina apresentou boa propriedade de estabilização da suspensão (RE % = 86,5) e em combinação com proteína de farelo do arroz possibilitou maior EE % (79,4). As microcápsulas exibiram diâmetro médio entre 3,4 a 4,6 µm e a morfologia das microcápsulas produzidas com a combinação da albumina sérica bovina e a proteína do farelo de arroz apresentaram superfícies esféricas com ausência de fissuras ou deformações. As análises térmicas e de FTIR, confirmam a eficiência de encapsulação do processo, indicando uma possível interação entre os agentes encapsulantes e o eugenol. / Eugenol is a natural phenolic compound with antioxidant and antimicrobial activity and its use as substitute the synthetic additives in food has been suggested. However, due eugenol instability to extern agents (light, oxygen and hot), its use in food processing has been hampered. Therefore, microencapsulation is a viable alternative for your application. The aims of this work were evaluate the effect of variation of operating conditions of spray drying (inlet air temperature and feed flow rate) in obtainment eugenol microencapsulated in carrageenan, and study the influence of combination of carrageenan and protein from rice bran protein, bovine serum albumin and, whey protein with low lactose content in the eugenol microencapsulation. Composite Central Desing (CCD) of type 22 with two independent variables (inlet air temperature, and feed flow rate), three key points and four axial points, were developed to assess the operational conditions of spray dryer. Eugenol quantification, recovery (% ER) and encapsulation efficiency (EE%) of process were evaluated by UV-Vis spectrophotometry and morphology by optical microscopy. In the second stage of the study, the influence of the use of carrageenan in combination with rice bran protein, bovine serum albumin and whey protein with low lactose content was evaluated by simplex-centroid desing. Microcapsules were characterizated by Ultra Performance Liquid Chromatography (UPLC) (ER and EE%), thermogravimetric analysis coupled to the infrared spectrophotometry, and morphology by scanning electron microscopy (SEM). In the CCD, the maximum ER% value was 12% and the operating conditions studied did not influence significantly (p > 0.05). EE% varied from 18.0 to 84.8% and the quadratic term to feed flow rate presented significant influence (p ≤ 0.05) in the evaluated answer. In the simplex-centroid mixture desing the ER% average of microcapsules ranged from 37.9 to 104.5% and EE% 0.0 to 79.4%, being that both responses were influenced (p ≤ 0.05%) by encapsulating agents of formulation. Bovine serum albumin presented good stabilizing property of suspension (ER% = 86.5) and in combination with rice bran protein resulted greater EE% (79.4). Microcapsules exhibited a average diameter range from 3.4 to 4.6 µm and the microcapsules morphology produced combination with the bovine serum albumin and protein rice bran showed surface with absence no cracks or deformation. Thermal and FTIR analysis confirmed the encapsulation efficiency of the process, observed a possible interaction between the encapsulating agents and eugenol.

O eugenol é um composto fenólico natural que apresenta atividade antioxidante e antimicrobiana e o seu uso como substituto de aditivos sintéticos em alimentos tem sido proposto. Contudo, pela sua instabilidade frente aos agentes externos (luz, oxigênio e calor), seu uso no processamento de alimentos é comprometido. Assim, a microencapsulação é uma alternativa viável para sua aplicação. Os objetivos deste trabalho foram avaliar o efeito da variação das condições operacionais do atomizador (temperatura do ar de entrada e vazão de alimentação) na obtenção de eugenol microencapsulado em carragena, e estudar a influência da combinação de carragena e proteína do farelo de arroz, albumina sérica bovina e proteína do soro de leite com baixo teor de lactose na microencapsulação de eugenol. Em uma primeira etapa, um Delineamento Composto Central Rotacional (DCCR) do tipo 22 com duas variáveis independentes (temperatura do ar de secagem e vazão de alimentação), três pontos centrais e quatro pontos axiais, foi desenvolvido para avaliar as condições operacionais de atomização. A quantificação do eugenol, recuperação (RE %) e a eficiência de encapsulação (EE %) foi avaliadada por espectrofometria UV-Vis e a morfologia por microscopia ótica. Na segunda etapa, a influência do uso de carragena em combinação com proteína do farelo de arroz, albumina sérica bovina e proteína do soro de leite com baixo teor de lactose foi avaliada por meio de um planejamento de mistura do tipo simplex-centroid. A caracterização das microcápsulas foi determinada pela RE % e EE % por Cromatografia Líquida de Alta Eficiência (CLAE), análise termogravimétrica acoplada à espectrofotometria de infravermelho e, morfologia por microscopia eletrônica de varredura. Para o DCCR, o valor máximo de RE% obtido foi de 12% e as condições operacionais estudadas não influenciaram significativamente (p > 0,05). Já a EE% variou de 18,0 a 84,8% e, o termo quadrático para vazão de alimentação apresentou influência significativa (p ≤ 0,05) na resposta avaliada. Para o planejamento simplex-centroid, o valor médio de RE % das microcápsulas variou de 37,9 a 104,5% e o de EE% de 0,0 a 79,4%, sendo que ambas as respostas foram influenciadas (p ≤ 0,05%) pelos agentes encapsulantes da formulação. A albumina sérica bovina apresentou boa propriedade de estabilização da suspensão (RE % = 86,5) e em combinação com proteína de farelo do arroz possibilitou maior EE % (79,4). As microcápsulas exibiram diâmetro médio entre 3,4 a 4,6 µm e a morfologia das microcápsulas produzidas com a combinação da albumina sérica bovina e a proteína do farelo de arroz apresentaram superfícies esféricas com ausência de fissuras ou deformações. As análises térmicas e de FTIR, confirmam a eficiência de encapsulação do processo, indicando uma possível interação entre os agentes encapsulantes e o eugenol. / Eugenol is a natural phenolic compound with antioxidant and antimicrobial activity and its use as substitute the synthetic additives in food has been suggested. However, due eugenol instability to extern agents (light, oxygen and hot), its use in food processing has been hampered. Therefore, microencapsulation is a viable alternative for your application. The aims of this work were evaluate the effect of variation of operating conditions of spray drying (inlet air temperature and feed flow rate) in obtainment eugenol microencapsulated in carrageenan, and study the influence of combination of carrageenan and protein from rice bran protein, bovine serum albumin and, whey protein with low lactose content in the eugenol microencapsulation. Composite Central Desing (CCD) of type 22 with two independent variables (inlet air temperature, and feed flow rate), three key points and four axial points, were developed to assess the operational conditions of spray dryer. Eugenol quantification, recovery (% ER) and encapsulation efficiency (EE%) of process were evaluated by UV-Vis spectrophotometry and morphology by optical microscopy. In the second stage of the study, the influence of the use of carrageenan in combination with rice bran protein, bovine serum albumin and whey protein with low lactose content was evaluated by simplex-centroid desing. Microcapsules were characterizated by Ultra Performance Liquid Chromatography (UPLC) (ER and EE%), thermogravimetric analysis coupled to the infrared spectrophotometry, and morphology by scanning electron microscopy (SEM). In the CCD, the maximum ER% value was 12% and the operating conditions studied did not influence significantly (p > 0.05). EE% varied from 18.0 to 84.8% and the quadratic term to feed flow rate presented significant influence (p ≤ 0.05) in the evaluated answer. In the simplex-centroid mixture desing the ER% average of microcapsules ranged from 37.9 to 104.5% and EE% 0.0 to 79.4%, being that both responses were influenced (p ≤ 0.05%) by encapsulating agents of formulation. Bovine serum albumin presented good stabilizing property of suspension (ER% = 86.5) and in combination with rice bran protein resulted greater EE% (79.4). Microcapsules exhibited a average diameter range from 3.4 to 4.6 µm and the microcapsules morphology produced combination with the bovine serum albumin and protein rice bran showed surface with absence no cracks or deformation. Thermal and FTIR analysis confirmed the encapsulation efficiency of the process, observed a possible interaction between the encapsulating agents and eugenol.