This thesis combines four manuscripts of which I am the first author. The first manuscript examines the phase separation process and related process parameters. This article provides detailed experimental results of the delivery and separation process. During the delivery of 40% Liquid-to-Powder-Ratio (LPR) paste, only 62[plus ou moins]3 % of the paste initially present in the 10-mL syringe could be injected. Thereafter, the remaining paste in the syringe was not amendable to injection suggesting the existence of liquid separation. The LPR of the extruded fraction of a 37% LPR paste ranged from 40.9[plus ou moins]2.0 % to 42.7[plus ou moins]2.1 %. On the other hand, a shortage of water content was measured for the paste left in the syringe. Furthermore, this shortage was gradual, ranging from 27.3[plus ou moins]1.9 % at the plunger side to 30.9[plus ou moins]1.6 % at the tip side. In addition, this article presents rheological measurements of the paste showing clearly that the limitation was not related to the viscosity of the paste but rather to the phase separation process. Specifically, the yield stresses were around 66[plus ou moins]2 Pa, 19[plus ou moins]2 Pa, and 8[plus ou moins]0 Pa for 40%, 50%, and 65% LPR suspensions, respectively. For the three studied LPRs, the viscosity rapidly dropped with an increase of shear rate to a level below 10 Pas. The second manuscript examines the possibility that fine particles migrate faster than large particles during injection, hence leading to a so-called size separation. This size separation process can be expected from the scientific literature, but had not been investigated prior to my study. In a way, the size separation is very similar to the phase separation process. An electrohydraulic system was used to control the delivery process. The result of this second study, showed no evidence of size separation. It was therefore concluded that the main mechanism underlying the limited injectability is the liquid phase filtration through the porous particles bed of the paste. The third manuscript examines the role of powder porosity ([epsilon]) and permeability. For that purpose, an electronically assisted device was used to measure the powder permeability. In this study, three powders were examined for comparison and better understanding. In addition, the powder permeability was correlated with the paste injectability. Adding 3 wt% of a fine nanosized powder to the [bêta]-TCP powder decreased the mixture permeability at a porosity of [varepsilon] = 67.5% from 6.4.10[exposant]-13 m[exposant]2 to 5.6.10[exposant]-13 m[exposant]2 and increased the injected volume fraction from 70.8[plus ou moins]1.9 % to 84.5[plus ou moins]0.9 %. The results showed clear evidence that the injectability can be improved by admixing different powders. However, permeability was not a strong predictor of the liquid separation phenomenon. The last manuscript provides a practical solution to reduce phase separation occurrence. For that purpose an ultrasonication process was suggested and applied during the delivery process to improve injectability. Specifically, sonicating the paste reduced agglomeration, decreased paste viscosity due to the shear thinning and therefore reduced phase separation. The result of the ultrasound assisted delivery was remarkably effective since it has been able to fully deliver highly concentrated paste, with minimal force exerted by hand. For instance, the injectable volume fraction of a 40% LPR paste injected with a 5-mL syringe increased significantly from 71.3[plus ou moins]0.5 % to 99.1[plus ou moins]0.9 % using 150 microns ultrasonic amplitude at a 20 kHz frequency. This chapter provides clear evidence that an electromechanical approach can be used to improve the injectability of a calcium phosphate paste. This thesis addresses an important limitation of calcium phosphate cements, namely phase separation during injection. This thesis also provides a scientific understanding and a practical solution for this problem. The electromechanical solution proposed here is one out of several possible solutions. Future work may focus on building numerical tools to help in the design of the powder and to understand the link between powder properties, rheology, syringe geometry and phase separation."--Résumé abrégé par UMI

Extraction of fructo-oligosaccharide syrups from grated jerusalem artichoke (JA) tubers was studied by water at 20-60&deg / C by determining the yield, degree of polymerization (DP), product profile (DP of up to 6) and prebiotic effect using Lactobacillus plantarum on samples harvested between October and April, stored for 0-20 days. The optimum solvent to solid ratio was 4, the duration of shaking water bath extraction was 40 min and yield based on JA were 12-17%. Temperature was found to improve yield and functionality, and citric acid, at 26 mM, improved the color and darkness by 70 and 80%, respectively. Short-time (1 min) microwaving prior to extraction increased the yield by about 20%, decreased the amount of sugars with DP 1 and 2 and increased the amounts of oligosaccharides (OS) with DP 3-6, although the prebiotic effect increased only slightly / while the color and darkness of the syrup were tripled. Ultrasound-assisted-extraction (USE) gave best performance at 3 min duration / decreased the amounts of sugars with DP 1-2, increased the amounts of OS with DP 3-6, with 18% decrease in the yield. The better functionality of USE syrups were also indicated by 2.5 times higher growth rate of L.plantarum. The application of USE at 60&deg / C compared to 20&deg / C almost tripled the amounts of functional sugars. In order to obtain the largest proportion of monosaccharide units as functional sugars, 10 day storage at 4&deg / C after harvest was indicated. Ultrasonication did not affect the color but the darkness was doubled. The density and viscosity of all the syrups were practically the same.

This paper presents the fabrication of controlled release devices for anticancer drug paclitaxel using supercritical antisolvent method. The thermodynamic and hydrodynamic effects during supercritical antisolvent process on the particle properties obtained were investigated. Scanning electron microscopy was employed to study particle sizes and morphologies achieved. It was observed that increasing supercritical pressure improves the surface morphology of particles obtained, and increasing the flow rate of the organic solution jet reduces the particle sizes obtained. A modified Supercritical Antisolvent with Enhanced Mass transfer setup was developed to produce monodispersed nanoparticles with high recovery yield. High performance liquid chromatography was used to determine the encapsulation efficiency and in vitro release profiles of paclitaxel loaded particles obtained. The encapsulation efficiencies of particles obtained using the modified SASEM process were high and up to 83.5%, and sustained release of paclitaxel from the polymer matrix was observed over 36 days release. The thermogram properties of the particles were also analyzed using differential scanning calorimetry to determine the crystalline state of polymer and drug. / Singapore-MIT Alliance (SMA)

The main objective of the study was to encapsulate the phenolic compounds from sour cherry pulp in micro size, to investigate the physicochemical properties of capsules and their digestability in simulated gastric and intestinal fluid. The effect of different coating materials, ultrasonication time and core to coating ratio on encapsulation of phenolic compounds from sour cherry pomace was investigated. Maltodextrin and gum Arabic were chosen as coating materials. Coating material was prepared with different maltodextrin:gum Arabic (MD:GA) ratios of 10:0, 8:2, 6:4 to make the total solid content 10%. In addition, two different core to coating ratios of 1:10 and 1:20 were used. Emulsions were prepared by homogenization through ultrasonication at 160 W power and 20 KHz frequency for different time periods (5-30 min). Then, the emulsions were freeze dried for 48 hours to obtain the microcapsules. Encapsulation efficiency, antioxidant activity, surface morphology, particle size, color, digestability and glass transition temperatures of the microcapsules were determined. The microcapsules with a core to coating ratio of 1:20 were found to have higher encapsulation efficiencies (78.80-92.26%) than those with a core to coating ratio of 1:10 (69.38-77.83%). Increasing the gum Arabic ratio in the coating material increased encapsulation efficiency. Optimum conditions for encapsulation with the highest efficiency and the lowest particle size were sonication time of 22.5 min, MD:GA ratio of 8:2 and core to coating ratio of 1:20. Encapsulation was effective in preventing the release of the phenolic compounds in gastric fluid. On the other hand, phenolic compounds were released from the capsules into the intestinal fluid.

ABSTRACT ENCAPSULATION OF WHEAT GERM OIL Yazicioglu, Basak M.Sc., Department of Food Engineering Supervisor: Prof. Dr. Serpil Sahin Co- Supervisor: Prof. Dr. G&uuml / l&uuml / m Sumnu February 2013, 82 pages Wheat germ oil is a rich source of omega 3 and omega 6, octacosanol and tocopherol which has vitamin E activity. Due to these properties it is beneficial for health but it is prone to oxidation in free form. The aim of this study was to encapsulate wheat germ oil in micron size and determine the best encapsulation conditions by analysing encapsulation efficiency, particle size distribution and surface morphology of the capsules. The effects of core to coating ratio, coating materials ratio and ultrasonication time on encapsulation of wheat germ oil were investigated. Maltodextrin (MD) and whey protein concentrate (WPC) at different ratios (3:1, 2:2, 1:3) were used as coating materials. Total solid content of all samples was 40% (w/w). Five different core to coating ratios (1:8, 1:4, 2:4, 3:4, 4:4) were experimented. Ultrasound was used at 320 W and 20 kHz frequency for three different times (2, 5, 10 min). Prepared emulsions were frozen and then freeze dried for 48 hours to obtain microcapsules. Encapsulation efficiency analysis, particle size analysis and scanning electron microscopy (SEM) analysis were performed. Increasing WPC content in coating led to an increase in encapsulation efficiency. Microcapsules prepared with MD:WPC ratio of 1:3 were found to have higher encapsulation efficiencies (65.62%-89.62%) than the other ratios. Increase in oil load led to decrease in encapsulation efficiency thus 1:8 core to coating ratio gave better results. The best conditions for microcapsules were determined as ultrasonication time 10 min, core to coating ratio of 1:8 and MD:WPC ratio 1:3.

Through past research, it is known that carbon nanotubes have the potential of enhancing the thermal performance of heat transfer fluids. The research is of importance in electronics cooling, defense, space, transportation applications and any other area where small and highly efficient heat transfer systems are needed. However, most of the past work discusses the experimental results by focusing on the effect of varying concentration of carbon nanotubes (CNTs) on the thermal performance of CNT nanofluids. Not much work has been done on studying the effect of processing variables. In the current experimental work, accurate measurements were carried out in an effort to understand the impact of several key variables on laminar flow convective heat transfer. The impact of ultrasonication energy on CNT nanofluids processing, and the corresponding effects on flow and thermal properties were studied in detail. The properties measured were viscosity, thermal conductivity and the convective heat transfer under laminar conditions. Four samples of 1 wt % multi walled carbon nanotubes (MWCNT) aqueous suspensions with different ultrasonication times were prepared for the study. Direct imaging was done using a newly developed wet-TEM technique to assess the dispersion characteristics of CNT nanofluid samples. The results obtained were discussed in the context of the CNT nanofluid preparation by ultrasonication and its indirect effect on each of the properties. It was found that the changes in viscosity and enhancements in thermal conductivity and convective heat transfer are affected by ultrasonication time. The maximum enhancements in thermal conductivity and convective heat transfer were found to be 20 % and 32 %, respectively, in the sample processed for 40 minutes. The thermal conductivity enhancement increased considerably at temperatures greater than 24 °C. The percentage enhancement in convective heat transfer was found to increase with the axial distance in the heat transfer section. Additionally, the suspensions were found to exhibit a shear thinning behavior, which followed the Power Law viscosity model.

The primary objective of this study was to obtain nano-emulsion containing polyphenolic compounds extracted from sour cherry pomace and to investigate the effect of degritting of polyphenolic concentrates on the encapsulation efficiency and particle size distribution of capsules and emulsions. It was also aimed to study storage and baking stability of the capsules. Extracted polyphenolic concentrate was degritted at 10,000 rpm for 2 min. Purification reduced Sauter mean diameter (D[32]) of concentrated extract from 5.76 &mu / m to 0.41 &mu / m. Unpurified and purified concentrates were freeze dried for 48 h to obtain extracted phenolic powder (EPP) and purified extracted phenolic powder (PEPP), respectively. Powders were entrapped in two types of coating materials which contain 10% maltodextrin (MD) or 8% MD-2% gum arabic (GA). Samples were prepared by ultrasonication (160 W, 50% pulse) for 20 min. Emulsions containing EPP had D[32] of 1.65 and 1.61 &mu / m when they were entrapped in 10% MD and 8% MD-2% GA coating material solutions, respectively. It was possible to obtain nano-emulsions when purification step was performed. Emulsions prepared with PEPP and coated with 10% MD and 8% MD-2% GA had D[32] of 0.396 and 0.334 &mu / m, respectively. Encapsulation efficiency of the capsules increased significantly from 86.07-88.45% to 98.01-98.29% by means of degritting (p&le / 0.001). Loss of total phenolic content during storage at 43% and 85% relative humidities was smaller for encapsulated powders when compared to powders not entrapped in coating material. In addition, encapsulation significantly increased retention of phenolic compounds from 15.1-22.2% to 30.4-30.7% during baking (p&le / 0.05).

Grape pomace is a by-product of wineries. It is one of the most potent antioxidant sources due to its high phenolic content. In this thesis study, ultrasound assisted extraction of phenolic compounds from Merlot grape pomace has been studied. The effects of sonication time, subsequent extraction time in shaking water bath at 45&deg / C and composition of the solvent on extraction efficiency and recovery of phenolics were studied by response surface methodology. Folin-Ciocalteu colorimetric method was used to analyze effects of process parameters on the total phenolic content of the extracts. The best recovery (47.2 mg gallic acid equivalents of total phenolics per g of dried grape pomace) was obtained using 30 % aqueous ethanol and applying 6 minutes of sonication followed by 12 minutes of shaking in water bath at 45&deg / C.

Orientadora: Prof. Dra. Márcia Aparecida da Silva Spinacé / Dissertação (mestrado) - Universidade Federal do ABC, Programa de Pós-Graduação em Nanociências e Materiais Avançados, 2016. / Nos ultimos anos, varios metodos tem sido desenvolvidos para obtencao de nanocristais de celulose. Dentre eles, destaca-se o por ultrassom de alta intensidade, utilizado neste trabalho para fibra de bambu. Foram avaliadas diferentes condicoes de extracao de celulose por ultrassom, alterando tempo de reacao, densidade de massa e de potencia em relacao ao volume e tipo de pre tratamento. As amostras foram caracterizadas por microscopia optica, teor de umidade, espectroscopia de infravermelho, microscopia eletronica de varredura, espalhamento de luz dinamico, microscopia de forca atomica, analise termogravimetrica e difracao de raio X. A fibra de partida apresentou razao de aspecto de 2,33, com comprimento medio de 35 ¿Êm e diametro medio de 15 ¿Êm. Os nanocristais obtidos apresentaram dimensao entre 3 nm a 1 ¿Êm, com geometria elipsoidal. Concluiu-se que maior densidade de potencia e maior quantidade de massa conferiram maior reprodutibilidade ao processo e maior grau de cristalinidade a amostra (75 %), sendo indicado para aplicacao em nanocompositos polimericos . / In the last years, a lot of methods have been developed to obtain cellulose nanocrystals. Among them, there is high intensity ultrasound, used in this work to bamboo fiber. Different conditions of extraction of cellulose by ultrasound were evaluated, changing reaction time, mass and power density in relation to volume and pretreatment type. The samples were characterized by optics microscopy, moisture content, infrared spectroscopy, scanning electronic microscopy, dynamic light scattering, atomic force microscopy, thermogravimetric analysis and X ray diffraction. The original fiber showed aspect ratio of 2,33, with medium length of 35 ìm and medium diameter of 15 ìm. The nanocrystals showed dimensions between 3 nm and 1 ìm, with ellipsoidal geometry. It was observed that higher power density and higher mass allow better reproducibility of the process and higher crystallinity to the sample (75 %), it is indicated to applications in polymeric nanocomposites.

This work deals with the use of inorganic nanofibers in refractory castables. The thesis describes some of the results of previously conducted research on nanofibers. Also description of nanofibres, production and distribution. The experimental part is focused on studying the interaction of Al2O3 and SiO2 nanofibres with aluminate cement. The main subject of investigation is a dispersion of nanofibers using a surfactant and ultrasonication.