A Chamomilla recutita L. é uma das plantas medicinais mais cultivadas no Brasil e no mundo. Os extratos da C. recutita são de interesse para as indústrias farmacêuticas e cosméticas, visto que estes apresentam atividades anti-inflamatória, antioxidante e adstringente. A ação terapêutica do extrato pode ser mais pronunciada que a ação terapêutica de um de seus ativos isolados. No entanto, a incorporação de um extrato em uma formulação pode ser difícil devido à baixa estabilidade dos extratos, bem como à possibilidade de gerarem instabilidade das formulações. Microencapsulando o extrato com um carreador é possível aumentar estabilidade do extrato quanto evitar instabilidade na formulação. Além disso, a microencapsulação é capaz de fornecer outras vantagens, como uma liberação controlada. Dois processos foram estudados como alternativas para a microencapsulação do óleo essencial e do extrato hidroalcoólico da C. recutita usando quitosana como carreador: o spray drying e o spray freeze drying. Planejamentos fatorais foram utilizados para determinar os fatores que mais influenciaram no diâmetro médio das micropartículas, eficiência de encapsulação e teor dos marcadores e rendimento do processo. A apigenina e a apigenina-7-glicosídeo foram usadas como marcadores do extrato hidroalcoólico e o óxido de bisabolol A foi usado como marcador do óleo essencial. Os processos de spray drying e spray freeze drying dos dois extratos foram otimizados e as micropartículas resultantes foram caracterizadas com relação ao diâmetro médio, rendimento do processo, teor e eficiência de encapsulação dos marcadores, atividade antioxidante in vitro, densidade, índice de Carr, fator de Hausner, umidade, morfologia, perfil de liberação n vitro e estabilidade. Os resultados mostraram que o processo de spray drying apresentou os melhores resultados para eficiência de encapsulação, com valores de aproximadamente 98%, 95% e 80% para apigenina, apigenina-7-glicosídeo e óxido de bisabolol A, respectivamente. As eficiências de encapsulação obtidas no processo de spray freeze drying foram de aproximadamente 59%, 58% e 38% para os mesmos marcadores, respectivamente. As micropartículas produzidas por spray freeze drying apresentaram formato irregular e poroso, enquanto as produzidas por spray drying apresentaram formato esférico e superfícies mais lisas, sem poros ou fissuras. Ao contrário do que ocorreu com o extrato hidroalcoólico, a perda do marcador do óleo foi elevada no processo de spray drying, com teor final de 35%. Os teores dos marcadores ficaram acima de 80% para o processo de spray freeze drying do óleo e acima de 90% para o extrato hidroalcoólico. As micropartículas produzidas por spray drying do extrato hidroalcoólico e do óleo e por spray freeze drying do extrato hidroalcoólico e do óleo apresentaram diâmetro médio de 5,1 ?m, 5,0 ?m, 31,0 ?m e 96,4 ?m, respectivamente. Ensaios de liberação in vitro mostraram que as micropartículas foram capazes de sustentar a liberação dos respectivos marcadores. Os estudos de permeação in vitro das micropartículas produzidas por spray drying do extrato hidroalcoólico também mostraram que estas foram capazes de sustentar a liberação. A microencapsulação proporcionou em todos os casos um aumento considerável da estabilidade. As micropartículas produzidas por spray drying do extrato hidroalcoólico apresentaram teores de marcadores no mínimo 50% maiores que o extrato puro após 90 dias. O spray freeze drying se mostrou como a melhor alternativa para produção de micropartículas de quitosana contendo o óleo essencial de C. recutita, enquanto o processo de spray drying se mostrou como uma ótima alternativa para microencapsulação do extrato hidroalcoólico da C. recutita. / Chamomilla recutita L. is one of the most cultivated medicinal plants in Brazil and around the world. Its extracts are important to both the pharmaceutical and cosmetics industries due to its therapeutic applications, such as an anti-inflammatory, antioxidant, and astringent. The therapeutic effects of an extract may be more pronounced than those of an isolated active compound. However, the incorporation of an extract in a formulation is difficult due to the low stability of extracts and the potential instabilities they may cause in formulations. Microencapsulating an extract in a carrier is a potential way of increasing the stability of an extract and avoiding instabilities in a formulation. Compound microencapsulation also brings other advantages, such as controlled release rates. Two processes were studied as alternatives to microencapsulating C. recutita essential oil and C. recutita hydroalcoholic extract using chitosan as a carrier: spray drying and spray freeze drying. Factorial designs were used to determine which process factors most influence the mean diameter, encapsulation efficiency and content of the chemical markers, and process yield. Apigenin and apigenin-7-glucoside were used as chemical markers for the hydroalcoholic extract and bisabolol oxide A was used as the chemical marker for the essential oil. The spray drying and spray freeze drying processes for both the oil and hydroalcoholic extract were optimized and the resulting microparticles were further characterized to determine mean diameter, process yield, marker encapsulation efficiency and content, in vitro antioxidant activity, density, Carr index, Hausner factor, water content, morphology, in vitro release profiles and stability. The results showed spray drying had the best encapsulation efficiency results, with about 98%, 95% e 80% of the apigenin, apigenin-7-glucoside and bisabolol oxide A content, respectively, inside the microparticles. The encapsulation efficiencies obtained in the spray freeze drying process were about 59%, 58% e 38% for the same chemical markers, respectively. Microparticles produced by spray freeze drying were irregular and porous, whereas microparticles produced by spray drying were spherical and fairly smooth, without porous or cracks. Contrary to what happened with the hydroalcoholic extract, oil marker content was low for spray dried microparticles, with final content at 35%. Chemical markers contents were above 80% for the oil and above 90% for the hydroalcoholic extract in spray freeze dried microparticles. Spray dried microparticles containing extract and oil and spray freeze dried microparticles containing extract and oil had mean diameter of 5.1 ?m, 5.0 ?m, 31.0 ?m and 96.4 ?m, respectively. In vitro release profiles showed all microparticles were able to sustain their respective marker release rates. In vitro permeation studies of spray dried microparticles containing hydroalcooholic extract also showed sustained release rates for the corresponding markers. Microencapsulation also provided considerable increase in C. recutita hydroalcoholic extract stability and C. recutita essential oil stability. After 90 days spray dried microparticles containing hydroalcoholic extract presented marker content 50% higher than the pure hydroalcoholic extract. Spray freeze drying was the best alternative to produce chitosan microparticles containing C. recutita essential oil, while spray drying was shown to be an excellent way to microencapsulate C. recutita hydroalcoholic extract in chitosan.

Bien que représentant plus d’un quart de la distribution en énergie de notre Univers ainsi que la majorité (84\%) de la masse de celui-ci, la nature de la matière noire n’a pas encore été percée à ce jour. Dans cette thèse, il sera supposé que la matière noire est une nouvelle particule élémentaire, stable et dont la connexion (hors interactions gravitationnelles) avec le secteur visible est réalisée grâce à une autre particule, le médiateur. Au sein de ces lignes, la matière noire sera supposée être un fermion de Dirac et le médiateur un boson (vecteur ou scalaire), ce dernier étant choisi comme étant plus léger que la matière noire. Cette thèse propose d’explorer les aspects infrarouges de la production de la matière noire dans l’Univers primordial, le potentiel de détection d’une importante classe de candidats dits \enquote{freeze-in}, caractérisés par de très faibles interactions avec le Modèle Standard, auprès des expériences de détection directe et l’effet des auto-interactions de la matière noire sur son comportement superfluide dans les régions de haute densité de matière noire (halos, capture par des astres compacts) asymétrique. Sous ces hypothèses, premièrement, une étude exhaustive des différents mécanismes de production de la matière noire est réalisée, illustrée dans un modèle où le médiateur est un photon du secteur caché, issu d’un nouveau groupe de jauge U(1)’, qui mélange de façon cinématique avec le photon du Modèle Standard. En particulier, de nouveaux canaux de production sont mis en avant, nommément \textit{freeze-in from mediator} et \textit{sequential freeze-in}. Ceux-ci correspondent à des scénarios où la matière noire est très faiblement couplée au Modèle Standard, n’atteint jamais l’équilibre avec celui-ci dans l’Univers primordial et est produit petit à petit par des annihilations de médiateurs (en équilibre ou non avec le Modèle Standard). Il est ensuite montré que pour l’important et très attractif cas d’une matière noire milli-chargée (ainsi que pour des scénarios où le médiateur n’est pas plus massif que 40 méga-electronvolt), l’expérience de détection indirect Xenon1T contraint aujourd’hui l’espace des paramètres de la phase de freeze-in de ces modèles, et est, dans cette région de l’espace des paramètres, la contrainte la plus importante. Une réinterprétation des limites sur les interactions indépendantes du spin matière noire – nucléon est par ailleurs nécessaire, détaillée et validée. Dans la seconde partie de la thèse, l’effet des auto-interactions dans les scénarios de matière noire asymétrique est exploré. Sous l’hypothèse qu’un halo (galactique ou non) de matière noire atteint l’équilibre thermodynamique à très basse température (comparée à sa masse) et développe donc un potentiel chimique fini, des interactions matière noire – matière noire au voisinage de la surface de Fermi peut entraîner la formation de condensats, de transitions de phase du milieu et dès lors modifier drastiquement l’équation d’état du halo. Un système d’équations auto-consistant pour les condensats est présenté et résolu numériquement. Ensuite, la thermodynamique du système de gaz interagissant est explorée. Finalement, les interactions gravitationnelles sont considérées et les configurations auto-gravitantes, prenant en compte l’ensemble des auto-interactions, sont déterminées et leurs aspects phénoménologiques sont explorés.Even though dark matter represents more than a quarter of the energy budget of our Universe and the majority (84\%) of its mass, the nature of dark matter has not yet been unravelled. In this thesis, it will be assumed that dark matter is a new elementary particle, stable and whose connection (on top of gravitational interactions) with the visible sector is realized through another particle, the mediator. In this thesis, dark matter will be assumed to be a Dirac fermion and the mediator will be a boson (either vector or scalar). This thesis proposes to explore infrared aspects of the production of dark matter in the primeval Universe, aspects of detection of the important class of feebly coupled \enquote{freeze-in} candidates at direct detection experiments and aspects of condensed matter physics such as superfluidity in region of high dark matter density (halos or inside compact objects such as neutron stars). Under these hypothesis, we will first detail an exhaustive study of the possible thermal mechanism of dark matter production, illustrated in a model where the mediator is a dark photon, arising from a new $U\left(1\right)'$ gauge group, which kinematically mixes with the Standard Model photon. In particular, new production channels are put forward, namely the \textit{freeze-in from mediator} and \textit{sequential freeze-in}. They correspond to scenarios where dark matter is very feebly coupled to the Standard Model, do not reach equilibrium with the visible sector thermal bath in the Early Universe and are slowly produced by mediator annihilations (in-equilibrium or not with the Standard Model). It is then showed that for the popular case of a millicharged dark matter ( and for scenarios in which the mediator mass is not bigger than $40$ mega electronvolt), the direct detection experiment XENON1T constrains today the freeze-in parameter space of such models and is the strongest constraint overall for such candidates. A recast of the bounds on spin-independent dark matter$-$nucleon interactions was needed and we validate our procedure against other recast. In the second part of this thesis, the effects of self-interactions in asymmetric dark mater scenarios are explored. Under the hypothesis that a dark matter halo reaches thermodynamic equilibrium at very low temperature (compared to its mass) and develops a finite chemical potential, dark matter$-$ dark matter interactions at the vicinity of the Fermi surface can lead to the formation of condensates, to phase transitions and therefore modify drastically the equation of state of the halo. A self-consistant set of equations for the condensates is presented and solved numerically. The thermodynamics of the interacting dark matter cloud is also explored. Finally, gravitational interactions are considered and self-gravitating configurations of halos, taking into account self-interactions, are determined and their phenomenological aspects is explored. / Doctorat en Sciences / info:eu-repo/semantics/nonPublished

Neonatal painted turtles (Chrysemys picta) spend their first winter inside the shallow, subterranean nest cavity where they completed embryogenesis. Consequently, hatchlings at high latitudes may be exposed to ice and cold during the winter. This study was undertaken to determine how long hatchlings withstand freezing at temperatures slightly below 0°C because tolerance for freezing has been proposed to be the key to survival by overwintering animals. A thermocouple was glued to the carapace of each hatchling. The animal was dipped in water to provide a site of nucleation of ice and was then placed into a glass jar that was partially immersed in a circulating bath at -2°C. Carapace temperature was monitored throughout the procedure. When a freezing exotherm was detected, timing of the freezing event began. Animals were maintained in a frozen state for 12-48 h prior to being warmed to room temperature. Of the 39 hatchlings, 22 did not survive, and mortality increased as the duration of freezing increased. Logistic regression indicates that no turtle would have survived in a frozen state for more than 54 h. These results indicate that hatchlings can survive only brief exposure to freezing of the body fluids. Thus, hatchlings cannot tolerate freezing during prolonged periods of cold.

Master of Science / Department of Civil Engineering / Kyle Riding / Concrete is most widely used material in construction industry, which is made up of cement, water and aggregates as its major ingredients. Aggregates contribute to 60 to 75 % of the total volume of concrete. The aggregates play a key role in the concrete durability. The U.S Midwest has many aggregates that can show distress in the field under freezing and thawing conditions. The objective of this research was to determine if the Test Method for the Resistance of Unconfined Coarse Aggregate to Freezing and Thawing, method CSA A23.2-24A, could be used to differentiate good from poor performing aggregates in concrete. In this study fifty one KDOT aggregates (including twelve ledge and thirty nine production samples) were tested for freeze thaw resistance using CSA A23.2-24A test method and were compared to the results of the standard KDOT aggregate qualification tests. In addition to performing the CSA test method using a 3% sodium chloride solution, a subset of the aggregates were tested using either a 3% magnesium chloride or calcium chloride solution to determine the effects of the salt type on the aggregate performance. No correlation was found between the CSA A23.2-24A test method results and the standard KDOT aggregate qualification tests. The results also indicated that the mass loss in the CSA A23.2-24A was similar for the aggregate sizes tested. The use of alternate salt solutions like MgCl2 and CaCl2 resulted in increased freeze thaw mass loss in limestone aggregates.

Tesis por compendio / [ES] La industria alimentaria ha mostrado un enorme interés por desarrollar nuevos productos a base de fruta con el fin de satisfacer la demanda saludable y sostenible de productos alimentarios de los consumidores. En este sentido, un puré de naranja liofilizado podría representar una opción viable. La liofilización del puré da lugar a una torta que puede consumirse directamente como snack, o puede triturarse para obtener un polvo que puede utilizarse para una amplia gama de aplicaciones. Una optimización adecuada de las condiciones de liofilización podría ayudar a reducir su duración sin afectar a las características del producto final. Sin embargo, los alimentos deshidratados pueden presentar problemas de colapso estructural relacionados con su baja temperatura de transición vítrea. En este sentido, una técnica frecuente para la estabilización de estos productos deshidratados es la incorporación de biopolímeros de alto peso molecular. El objetivo de esta Tesis ha sido el diseño del proceso de liofilización para la obtención de un snack de naranja. Para ello se ha estudiado la influencia de diferentes combinaciones de biopolímeros en la estabilidad física del puré de naranja liofilizado (snack de naranja) y en la bioaccesibilidad in vitro de sus compuestos bioactivos. Asimismo, se ha evaluado su efecto en las propiedades de flujo en aire y de rehidratación del polvo de naranja. Se ha trabajado con diferentes combinaciones de goma Arábiga, maltodextrina, almidón sustituido por grupos octenil succínico, almidón nativo de maíz, fibras de guisante y de bambú. Los resultados mostraron la necesidad de incorporar estos biopolímeros para aumentar la actividad de agua crítica y el contenido de agua crítico para la transición vítrea, el cual se ha relacionado con la pérdida de la textura del snack. Si bien ninguna de las mezclas de biopolímeros fue mejor que las otras en higroscopicidad, carácter anti-plastificante, color y propiedades mecánicas del snack, la mezcla GA con FB fue la que mejoró la bioaccesibilidad de la vitamina C (VC) y de los compuestos fenólicos totales (TP). Además, esta misma combinación fue la que ofreció uno de los tiempos de mojado más cortos y una menor viscosidad del producto rehidratado, deseado para un producto tipo zumo. Por otra parte, se ha estudiado el impacto de las condiciones de liofilización en el consumo de energía del proceso y en la calidad del snack formulado con GA y FB. Las variables del proceso consideradas han sido la velocidad de congelación (convencional y abatidor), la temperatura de bandeja (30, 40, 50 ºC) y presión de trabajo (5, 100 Pa) durante el secado. Menor presión y mayor temperatura promovieron un ligero mayor secado de las muestras, obteniendo un producto más crujiente, con un color amarillo menos intenso, mejor preservación de VC y ß-caroteno (BC), y una reducción significativa, de hasta un 75%, en el consumo de energía total durante el secado, debido a la reducción del tiempo del proceso. La velocidad de congelación no tuvo impacto significativo sobre ninguna de las propiedades evaluadas. Por tanto, las condiciones recomendadas para el secado por liofilización son 5 Pa de presión y 50 ºC como temperatura de bandeja. Por último, se evaluó la estabilidad física y de los compuestos bioactivos y actividad antioxidante del snack almacenado en bolsas zip, a 4 y 20 ºC, durante 6 meses, simulando condiciones domésticas de almacenamiento. Como resultado, la muestra ganó cierta humedad, con la consecuente pérdida en porosidad y carácter crujiente a partir de los 2 meses. Asimismo, la luminosidad del snack almacenado a 20 ºC disminuyó pasados 2 meses, probablemente debido a las reacciones de pardeamiento, que incluyen la degradación de la VC (20%). BC sufrió una gran disminución, desde el inicio del almacenamiento y más cuanto mayor fue la temperatura. Por lo tanto, para este producto se recomienda un almacenamiento en refrigeración para una mejor preservación de los compuestos bioactivos. / [CA] La indústria alimentària ha mostrat un enorme interés per desenvolupar nous productes a base de fruita amb la finalitat de satisfer la demanda saludable i sostenible de productes alimentaris dels consumidors. En aquest sentit, un puré de taronja liofilitzat podria representar una opció viable. La liofilització del puré dona lloc a una coca que pot consumir-se directament com a snack, o pot triturar-se per a obtindre una pols que pot utilitzar-se per a una àmplia gamma d'aplicacions. Una optimització adequada de les condicions de liofilització podria ajudar a reduir la seua duració sense afectar les característiques del producte final. No obstant això, els aliments deshidratats poden presentar problemes de col·lapse estructural relacionats amb la seua baixa temperatura de transició vítria. En aquest sentit, una tècnica freqüent per a l'estabilització d'aquests productes deshidratats és la incorporació de biopolímers d'alt pes molecular. L'objectiu d'aquesta Tesi ha sigut el disseny del procés de liofilització per a l'obtenció d'un snack de taronja. Per a això s'ha estudiat la influència de diferents combinacions de biopolímers en l'estabilitat física del puré de taronja liofilitzat (snack de taronja) i en la bioaccessibilitat in vitro dels seus compostos bioactius. Així mateix, s'ha avaluat el seu efecte en les propietats de flux en aire i de rehidratació de la pols de taronja. S'ha treballat amb diferents combinacions de goma Aràbiga, maltodextrina, midó substituït per grups octenil succínic, midó natiu de dacsa, fibres de pésol i de bambú. Els resultats van mostrar la necessitat d'incorporar aquests biopolímers per a augmentar l'activitat d'aigua crítica i el contingut d'aigua crític per a la transició vítria, el qual s'ha relacionat amb la pèrdua de la textura del snack. Si bé cap de les mescles de biopolímers va ser millor que les altres en higroscopicitat, caràcter anti-plastificant, color i propietats mecàniques del snack, la mescla GA amb FB va ser la que va millorar la bioaccessibilitat de la vitamina C (VC) i dels compostos fenòlics totals (TP). A més, aquesta mateixa combinació va ser la que va oferir un dels temps de mullat més curts i una menor viscositat del producte rehidratat, desitjat per a un producte tipus suc. D'altra banda, s'ha estudiat l'impacte de les condicions de liofilització en el consum d'energia del procés i en la qualitat del snack formulat amb GA i FB. Les variables del procés considerades han sigut la velocitat de congelació (convencional i abatedor), la temperatura de safata (30, 40, 50 °C) i pressió de treball (5, 100 Pa) durant l'assecat. Menor pressió i major temperatura van promoure un lleuger major assecat de les mostres, obtenint un producte més cruixent, amb un color groc menys intens, millor preservació de VC i ß-caroté (BC), i una reducció significativa, de fins a un 75%, en el consum d'energia total durant l'assecat, a causa de la reducció del temps del procés. La velocitat de congelació no va tindre impacte significatiu sobre cap de les propietats avaluades. Per tant, les condicions recomanades per a l'assecat per liofilització són 5 Pa de pressió i 50 °C com a temperatura de safata. Finalment, es va avaluar l'estabilitat física i dels compostos bioactius i activitat antioxidant del snack emmagatzemat en bosses zip, a 4 i 20 °C, durant 6 mesos, simulant condicions domèstiques d'emmagatzematge. Com a resultat, la mostra va guanyar una certa humitat, amb la conseqüent pèrdua en porositat i caràcter cruixent a partir dels 2 mesos. Així mateix, la lluminositat del snack emmagatzemat a 20 °C va disminuir passats 2 mesos, probablement a causa de les reaccions de enfosquiment, que inclouen la degradació de la VC (20%). BC va patir una gran disminució, des de l'inici de l'emmagatzematge i més com més gran va ser la temperatura. Per tant, per a aquest producte es recomana un emmagatzematge en refrigeració per a una millor preservació dels compostos bioactius. / [EN] Food industries have showed a huge interest in developing new fruit-based products to satisfy the healthy and sustainable demand of food products by consumers. In this sense, offering a freeze-dried orange puree could represent a feasible option. Freeze-drying the puree results in a cake that can be consumed directly as a snack, or it can be crushed to obtain a powder that can be used for a wide range of applications. A suitable optimisation of the freeze-drying conditions could help to reduce its duration without affecting the characteristics of the final product. However, dehydrated foods may present problems of structural collapse related to its low glass transition temperature. In this sense, an approach for the stabilisation of dehydrated products is the incorporation of high molecular weight biopolymers. The aim of this Thesis has been the design of the freeze-drying process to obtain an orange snack. The influence of different combinations of biopolymers on the physical stability of the freeze-dried orange puree (orange snack) and on the in vitro bioaccessibility of its bioactive compounds has been studied. Their effect on the air flow and rehydration properties of an orange powder obtained after crushing the snack has also been evaluated. Different combinations of gum Arabic, maltodextrin, starch substituted with octenyl succinic groups, native corn starch, pea and bamboo fibres were used. The results showed the need to incorporate these biopolymers to increase the critical water activity and the critical water content for the glass transition, which has been related to the loss of snack texture. Although none of the biopolymer combinations was better than the others in terms of hygroscopicity, anti-plasticising character, colour, and mechanical properties of the snack, the GA mixed with FB was the one that improved the bioaccessibility of vitamin C (VC) and total phenolic compounds (TP). This same combination offered the shortest wetting times and a lower viscosity of the rehydrated product, which is desirable for a juice-type product. Also, the impact of the freeze-drying conditions on the energy consumption of the process and on the quality of the snack formulated with GA and FB has been studied. The process variables considered were freezing rate (conventional and blast freezer), shelf temperature (30, 40, 50 ºC) and working pressure (5, 100 Pa) during drying. Lower pressure and higher temperature promoted a slightly higher drying of the samples, which resulted in a crispier product, as well as a less intense yellow colour. However, at the sensory level, there was no significant preference for any of the samples processed under the different conditions studied. In addition, VC and ß-carotene (BC) were better preserved under these conditions, conditions which significantly reduced, up to 75%, the total energy consumption during drying, due to the reduction of the process time. The freezing rate had no significant impact on any of the properties evaluated. Therefore, the recommended conditions for freeze-drying to maximise the preservation of bioactive compounds, with a lower energy consumption, while providing a snack perceived as a crispy product by consumers, are 5 Pa pressure and 50 ºC as shelf temperature. Finally, the physical stability and the stability of bioactive compounds and antioxidant activity of the snack stored in zip bags at 4 and 20 ºC for 6 months, simulating domestic storage conditions, was evaluated. As a result, a certain moisture gain of the sample was observed, with a consequent loss in porosity and crispness after 2 months. Also, the luminosity of the snack stored at 20°C decreased after 2 months, probably due to browning reactions, including degradation of VC (20%). BC suffered a large decrease, from the beginning of storage and more so the higher the temperature. Therefore, refrigerated storage is recommended for better preservation of the bioactive compounds of this product. / Silva Espinoza, MA. (2021). Design of the process of obtaining a freeze-dried orange puree. Formulation, freeze-drying variables, and storage conditions [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/170354 / TESIS / Compendio

The medium offering the greatest resistance to heat transfer from the freeze-drying shelf to the moving and subliming surface is the space between the flat shelf top and the concave vial bottom. The resistance to heat transfer can be greatly reduced by improving the thermal conductivity of the intervening space. Several heat transfer augmentation devices, including a multilayered corrugated aluminum quilt and a conformable fluid cushion device, which fill this gap are described. The devices are inexpensive and easy to use. Experimental data show that the resistance of the intervening space is reduced appreciably and the drying rate is greatly increased. The fluid cushion device is superior to the aluminum quilt as it reduces the consequences of spillage of solution and provides greater intervial uniformity among the same batch of vials. Drying times obtained in experiments with and without the fluid cushion device are compared here for different sizes and different types of vials. Product evaluation is conducted by measuring the reconstitution time and observing the product under a microscope. The solubilities of two univalent electrolytes, sodium chloride and potassium chloride, have been measured in eight cosolvent-water binary systems. The solubility of both the solutes has been found to be adequately described by the log-linear solubility equation, log S(m) = log S(w) + fσ. The rank order of the desolubilization slopes obtained for the electrolyte solutes is compared with the solubilization of nonelectrolyte solutes. These results indicate that a cosolvent which is most effective in solubilizing a nonelectrolyte is also most effective in desolubilizing an electrolyte. The solubility of oxacillin sodium in methanol-water mixtures has been determined at various temperatures ranging from +21 to -26 degrees centigrade. The data has been fitted to the log-linear relationship as proposed by Yalkowsky et. al. The heat of solution is determined using the van't Hoff equation and was found to be nearly constant at 1.2 Kcal/mole. There appears to be no dependency of the slope of the log S(m) vs. fraction cosolvent plot to the temperature. The data suggests that there is a polymorphic or amorphic transition of oxacillin at -14.5 degrees centigrade.

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Wastewater sludge is considered a valuable source of nutrients and energy. Freeze/thaw treatment is an efficient dewatering method for wastewater sludge management in First Nation communities located in cold climate conditions. Natural freeze/thaw is a simple, practical and low cost method, which can effectively dewater sludge. The objective of this research is to evaluate dewatering, nutrient recovery and organics separation of wastewater sludge originating from different wastewater treatment processes using freeze/thaw processing. The results of experiments showed the effectiveness of this method in sludge dewaterability and solubilisation of organics and nutrients. The sludge solid content increased by approximately 10-fold after treatment. It was effective in solubilisation of about 15.2%, 33.5% and 21.5% of total nitrogen, total phosphorus and total chemical oxygen demand to soluble one, respectively for the non-BNR sludge. However, anaerobic digestion of the solid cake post freeze/thaw treatment did not show enhanced methane yield compared with fresh sludge. / February 2017

This work focuses on improving video transmission quality over a mobile link. More specifically, the impact of buffering and link outages on the freeze probability of transmitted videos is studied. It introduces a new fluid flow model that provides an approximation of the freeze probability in the presence of play-out hysteresis. The proposed model is used to study the impact of two streaming buffer sizes over different possible combinations of outage parameters (data channel on/off times). The outcome of this thesis shows that outage parameters play a dominant role in freezing of streaming video content, and that an increase in these parameters cannot be easily compensated for by an increase in the size of the receiving buffer. Generally, in most cases when there is a variation in outage parameters, an increased buffer size has a negative impact on the freeze probability. To lower the probability of freeze during video playback over a weak mobile link, it is better to sacrifice resolution just to keep the video content playing. Similarly, shifting focus from off to on times brings better results than increasing buffer size.

Three-dimensional collagen/chitosan scaffolds fabricated by freeze-drying technique in 96-well polystyrene and PDMS plates were optimized during this study. Surface tension is, by and large, one of the most limiting factors in fabricating freeze-dried scaffolds in small format well plates. Traditionally, bowl-shaped top surfaces of collagen/chitosan scaffolds were common in polystyrene 96-well plate; whereas for PDMS 96-well plate, dome-shaped surfaces were formed. These surface tension phenomena are not desirable in cell studies especially during initial cell seeding. A combination of surface treatment and change of freeze-drying regime were developed to mitigate the surface tension problem in PS and PDMS 96-well plates respectively. Collagen/chitosan scaffolds of varying concentration and composition were experimented in both polystyrene and PDMS 96-well plates. Thin water film treatment with UV cross-linking was successfully used to eliminate meniscus in PS well plates; pre-cooling, on the other hand, was utilised to treat scaffold solutions in PDMS well plates. The resultant matrices all had flat top surfaces and average thickness of 1 mm. As expected, scaffolds with lower overall polymer concentration or, from a compositional perspective, scaffolds with high chitosan content generally had larger pores. Microscopic observation by multi-photon microscope was performed and chemical analyses were conducted to characterize the surface-treated scaffolds. In addition, scaffolds were tested in vitro using DLD-1 cells, hMSCs and fibroblasts for their biological performance. The purpose of this study was to address the problem of using small format culture wells for the fabrication of freeze-dried collagen-based scaffolds for studies of cell growth in 3D culture and in microfluidic perfusion bioreactors.