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Collapse temperature of freeze-dried carbohydrate solutions : effects of composition and moisture content.Tsourouflis, Spyros Panayiotis Constantinos January 1975 (has links)
Thesis. 1975. M.S.--Massachusetts Institute of Technology. Dept. of Nutrition and Food Science. / Bibliography: leaves 109-112. / M.S.
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Mitigation of Undesirable Flavor in Kefir Intended for Adjuvant Treatment of <i>Clostridioides difficile</i> InfectionKesler, Megan Kathleen January 2019 (has links)
No description available.
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Formulace lyofilizovaných tablet pro bukální aplikaci vakcín. / Formulation of freeze dried tablets for buccal application of vaccinesVuová, Ngoc Lien January 2021 (has links)
Charles University, Faculty of Pharmacy in Hradec Králové Department of: Pharmaceutical Technology Mentor: Doc. PharmDr. Zdeňka Šklubalová, Ph.D. Student: Ngoc Lien Vuová Title of Thesis: Formulation of freeze dried tablets for buccal application of vaccines Mucosal vaccines represent an attractive way of vaccination with an advantage of inducing both systemic and local immunity. The aim of this diploma thesis was designing a composition of freeze-dried tablets for buccal administration of a model Bordetella pertusis vaccine. The easy removal from blister, firmness and aesthetic appearance as well as the appropriate taste and mucoadhesivity were the required product quality parameters. The excipients were characterised by differential scanning calorimetry, osmolality and pH measurement; the mechanical properties and disintegration time of freeze-dried tablets were evaluated. Among the variety of studied excipients and their combinations, dextran 40 as the main component of the preparation provided the best results. For the further modification of properties, the addition of fish gelatin, iota carrageenan and macrogol 300 is suitable. Freeze-dried tablets containing trehalose, mannitol and povidon 25 did not achieve the desirable quality parameters. Freeze- dried tablets containing iota carrageenan...
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Development of a Freeze-Drying Strategy to Store Human Bone Marrow Mesenchymal Stem/Stromal Derived Extracellular Vesicles for Applications in StrokeDorus, Brian 25 January 2023 (has links)
Mesenchymal stem/stromal cells (MSCs) release Extracellular vesicles (EVs) that are believed to play a major role in nerve regeneration after stroke. However, a major complication when trying to transition MSC-EVs from a pre-clinical to clinical setting is the convenient long-term storage of MSC-EVs. Therefore, we developed a strategy to freeze dry MSC-EVs to store them for more practical clinical applications. We first determined the optimal trehalose concentration for freeze drying the MSC-EVs, and we subsequently investigated the optimal freezing conditions. It was determined that 100 mM of trehalose and freezing temperature at -20°C were the optimal conditions to freeze dry the EVs. The therapeutic capabilities of the freeze-dried MSC-EVs was tested via tube formation assay and co-culturing them with neural stem/progenitor cells (NSPCs). It was found that human vein umbilical endothelial cells (HUVECs) treated with rehydrated MSCEVs promoted tube formation suggesting the trophic factors in the MSC-EVs survived the freeze-drying process. As for the NSPC co-culture, all treatments involving rehydrated MSC-EVs protected by trehalose during the freeze-drying process promoted proliferation and did not affect their ability to differentiate into oligodendrocytes, astrocytes, or neurons. Determining the optimum freezing-drying conditions allows us to stockpile a large amount of MSC-EVs at room temperature for on-demand applications.
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Use of Volumetric Heating to Improve Heat Transfer During Vial Freeze-DryingDolan, James Patrick Jr. 28 September 1998 (has links)
Freeze-drying (lyophilization) is a drying process which is used to remove water from heat sensitive products, usually for the purpose of preservation. By removing water, the product becomes more stable at room temperature. This is a common process in the pharmaceutical industry because freeze-drying offers the advantage of drying at low temperatures and producing very low residual moisture contents. Often the materials dried in this manner are heat sensitive and require the highest possible quality. However, freeze-drying is a very slow process, often requiring 24 to 48 hours. During the process, vacuum pumps and refrigeration systems run continuously, making freeze-drying a very expensive process.
The goal of this project was to show that volumetric heating can be used in pharmaceutical freeze-drying and that this mode of heating offers some advantages. There were two approaches taken to the work, one experimental and one analytical. The experimental approach was broken into two phases, one focused on comparing microwave and conventional freeze-drying and the other focused on demonstrating the advantages of volumetric heating. In the analytical approach, a mathematical model was used to confirm the trends observed in phase II of the experimental work.
Experiments were conducted in a conventional laboratory freeze-dryer and the drying rate results were compared to the results obtained with an experimental microwave freeze-drying apparatus. Experiments were also conducted with the vaccine strain <i>A. pleuropneumoniae</i>. A viability study was conducted, comparing the viability loss caused by each process. The viability study showed a slightly higher viability loss for the microwave process.
A comparison of drying curves showed that the microwave process resulted in a slight improvement in primary drying time: 2.5 hours for the microwave process compared to 3 hours for the conventional process. There was a significant difference in overall drying times: 4 hours for the microwave process compared to 11 hours for the conventional process. This result was caused by a lower residual moisture content at the start of secondary drying and a higher secondary drying temperature for the microwave process.
Experiments were also conducted to show that using lower chamber pressure results in higher drying rates. This is not the case in a conventional freeze-dryer since heating is dependent on the chamber pressure in the low pressure environment of freeze-drying. Thus, an advantage of volumetric heating was demonstrated. The results show that a modest increase in pressure, from 0.05 to 0.3 Torr, caused a one third reduction in primary drying time.
The mathematical model developed in the analytical work relied on the D'Arcy equation to describe the flow of vapor in the porous dried layer. The results of the model confirm trends seen in the measured temperature and weight profiles. Analyzing the effect of varying the chamber pressures shows that lowering the pressure in the range of 1 to 0.01 Torr results in a significant increase in drying rate giving as much as a two thirds reduction in drying time for the case studied. A model incorporating mass transport equations derived from the dusty gas model was also presented. This model offers the benefit of a more accurate prediction of mass transport through the porous dried layer.
NOTE: (09/2008) An updated copy of this ETD was added after there were patron reports of problems with the file. / Ph. D.
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Méthodes innovantes de séchage de suspensions de nanocristaux / Innovative methods to dry nanocrystalline suspensionsTouzet, Antoine 12 July 2018 (has links)
Les nouvelles molécules thérapeutiques présentent la plupart du temps une faible solubilité aqueuse, à l’origine d’une biodisponibilité restreinte lors de leur administration orale. La réduction de taille des cristaux de substance active à l’échelle submicronique (= production de nanocristaux) s’est imposée comme une voie majeure de formulation au cours de ces dernières années.Afin de pallier des problèmes d’instabilité et d’aboutir à des formes solides pratiques d’utilisation pour les patients, une étape de séchage est généralement effectuée après production des nanocristaux en suspension. L’objectif principal de cette étape est de générer un produit présentant à la fois des propriétés facilitant le déroulement d’étapes procédés avales mais aussi et surtout de prévenir l’agrégation des nanocristaux au risque de compromettre leur dissolution après administration.Plusieurs techniques sont aujourd’hui utilisées dans l’industrie pharmaceutique telle que l’enrobage/granulation en lit d’air fluidisé et le spray drying. Parallèlement à l’élaboration d’une « formulation standard » pour ces deux méthodes de référence, deux techniques innovantes de lyophilisation ont été investiguées dans ce travail. La stabilisation de nanocristaux de kétoconazole par cryopelletization et active freeze drying a été démontrée et les paramètres clefs identifiés. Les produits générés par ces deux techniques, respectivement sous forme de pellets ou de poudre fine, ont été comparés à ceux conçus par enrobage en lit d’air fluidisé et spray drying. En conclusion, ces travaux indiquent que la cryopelletization et l’active freeze drying se positionnent comme des procédés d’intérêt de seconde intention, permettant de traiter des cas particuliers (molécules sensibles au stress thermique, à l’humidité et/ou couteuses). / Newly active pharmaceutical ingredients very often suffer from low aqueous solubility, a fact that in many cases can lead to poor oral bioavailability. Nanosizing, referring to drug nanocrystals production by size reduction, has demonstrated over the past few years a great potential to overcome this major issue.Since solid oral dosage forms are generally preferred due to stability reasons and patient convenience, the production of nanocrystals in a liquid medium is usually followed by a drying step. The main objective of this drying step is to generate a product suitable for downstream processing operations while at the same time preventing nanocrystal aggregation which can adversely affect the dissolution performance of the dry product in vivo.Several drying techniques such as spray drying and coating/granulation in fluidized bed have been successfully implemented in the pharmaceutical industry. In this work, two innovative freeze drying techniques were investigated and compared to the two above mentioned reference methods. The suitability of cryopelletization and active freeze drying to stabilize ketoconazole nanocrystals has been demonstrated and the key process parameters identified. The formulations generated by these two innovative techniques in the form of pellets or fine powder particles, respectively, were compared to the previously manufactured by fluidized bed and spray drying. In conclusion, this work presents cryopelletization and active freeze drying as suitable second-line processes with potential to address the drying of formulations containing problematic molecules sensible to thermal stress, moisture and/or presenting high production costs.
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OBTENÇÃO DE COMPOSIÇÕES CERÂMICAS Mn-Ni-Co VIA SÍNTESE POR LIOFILIZAÇÃO E SUA CARACTERIZAÇÃO ELÉTRICA COMO SENSOR DE TEMPERATURA.Silva, Edson José Lima da 22 December 2011 (has links)
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Previous issue date: 2011-12-22 / This work describes the preparation of nanoparticles of spinel structure, made from oxides of Manganese, Nickel and Cobalt, via lyophilization process, which was compared to the process of obtaining conventional mixture of oxides, in order to analyze different forms of preparation and its influence on electrical properties (characteristic resistance, temperature coefficient, stability of the thermistor), through the measures obtained by applying a voltage of 5 volts on pads and subjecting them to a temperature range of 20 C to 300 C, measured with a thermocouple type K The microstructures were analyzed by scanning electron microscopy (SEM), the average particle size ranged from 60 to 93 nm. X-ray spectroscopy to determine the phases present in the samples and analysis of infrared to identify in the process, organic waste and the organic phase transitions were completely volatilized during the controlled heating pad on high-temperature furnace (with resistance molybdenum silicide) (Lindenberg). Through the obtained results it was noted a certain advantage at all temperatures of the samples had the composition Ni Mn and Co on the Mn Ni which had only giving larger values between 4335 and 4571 for samples made from the process liofilization. / Este trabalho descreve a preparação de nanoparticulas de estrutura espinélio, feitas a partir de óxidos de Manganês, Níquel e Cobalto, via processo de liofilização, o qual foi comparado ao processo de obtenção convencional, mistura de óxidos, afim de se analisar diferentes formas de preparação e sua influência nas propriedades elétricas (resistência característica, coeficiente de temperatura, estabilidade do termistor), através das medidas obtidas aplicando-se uma tensão de 5 volts nas pastilhas e submetendo-as a uma variação de temperatura de 20C a 300C, aferidos com um termopar tipo K. As Microestruturas foram analisadas por microscopia eletrônica de varredura (MEV), o tamanho médio das partículas ficaram entre 60 a 93 nm. Espectroscopia de raios X para determinação das fases presentes nas amostras e análise de infravermelho para se identificar em que fase do processo os resíduos orgânicos e as transições de fases orgânicas foram totalmente volatilizados ao longo do aquecimento controlado das pastilhas em forno de alta temperatura (com resistência de siliceto de molibdênio) (Lindenberg). Através dos resultados obtidos notou-se uma certa vantagem em todas as temperaturas das amostras que tinham na composição Mn Ni e Co sobre as que tinham apenas Mn Ni dando valores de maiores, entre 4335 e 4571 para as amostras feitas a partir do processo de liofilização.
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Design of the process of obtaining a freeze-dried orange puree. Formulation, freeze-drying variables, and storage conditionsSilva Espinoza, Marilú Andrea 17 June 2022 (has links)
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
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Application of through-vial impedance spectroscopy as a novel process analytical technology for freeze dryingArshad, Muhammad Sohail January 2014 (has links)
This study aims to validate and develop applications for a novel impedance-based process analytical technology for monitoring the attributes of the product during the entire freeze-drying process (from pre-freezing and annealing to primary and then secondary drying). This measurement approach involves the application of foil electrodes, mounted externally to a conventional glass freeze-drying vial, and coupled to a high-impedance analyser. The location of the electrodes on the outside, rather than the inside of the vial, leads to a description of the technology as a through-vial impedance spectroscopy (TV-IS) technique. The principle observation from this approach is the interfacial-polarization process arising from the composite impedance of the glass wall and product interface. For a conventional glass vial (of wall thickness ~ 1 mm and cross sectional diameter ~ 22 mm) it was shown that the process is manifest within the frequency range 101 to 106 Hz, as a single, broad band peak which spans 2-3 decades of the imaginary part spectrum. Features of the interfacial-relaxation process, characterised by the peak amplitude, C″Peak, and peak frequency, fpeak, of the imaginary capacitance spectra and the equivalent circuit elements that model the impedance spectra (i.e. the solution resistance (R) and solution capacitance (C) were monitored along with the product temperature data during the cycle(s), for a variety of surrogate formulations comprising lactose, sucrose, mannitol or maltodextrin solutions, during the freezing, re-heating, annealing and primary drying stages of freeze drying). It was shown that the parameters, fpeak and R, are strongly coupled to each other and change as a function of the temperature of the solution and its phase state, whereas C″Peak is strongly coupled to the amount of ice that remains during the drying process. Both log fpeak and log R have a linear dependence on the temperature of the solution, provided there was no phase change in the solution. The crystallization process (ice onset, solidification and equilibration to shelf temperature) is characterized well by both log fpeak and log R, whereas the parameter R demonstrates most clearly the formation of eutectic crystallization during freezing. In contrast it was the parameter C which was most sensitive to the detection of the glass transition during re-heating. During primary drying, it was shown that C″peak, is dependent on the amount of ice remaining and therefore provides a convenient assessment of the rate of drying and primary drying end point. The impedance changes during annealing provide a mechanistic basis for the modifications in ice structure which result directly in the observed decrease in primary drying times. The principal observation on annealing of a 10% w/v solution of maltodextrin, was the minimal changes in the glass transition (recorded at ~−16 °C) during the re-heating and cooling step (post-annealing). This result alone appears to indicate that a maximum freeze concentration was achieved during first freezing with no further ice being formed on annealing. The phenomenon of devitrification (and the production of more ice, and hence larger ice crystals) was therefore discounted as the mechanism by which annealing impacts the drying time. Having excluded devitrification from the mechanism of annealing enhanced drying, it was then possible to conclude that the decrease in the electrical resistance (that was observed during the annealing hold time) must necessarily result from the simplified structure of the unfrozen fraction and the improved connectivity of ice crystals that may be the consequence of Ostwald ripening. The application of through vial impedance measurement approach provides a non-invasive, real time monitoring of critical process parameters which subsequently leads to an improved understanding of the mechanisms and effects of different parameters, providing a reliable basis for process optimization, along with improved risk management to ensure optimum quality of the formulation and optimization of the freeze drying process.
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Synthesis and processing of nanostructured alumina ceramicsGhanizadeh, Shaghayegh January 2013 (has links)
The term Nanoceramics is well known in the ceramic field for at least two decades. In this project a detailed study was performed on the synthesis of α-alumina nanopowders. High solids content nanoalumina suspensions were prepared and used to form green bodies using both wet and dry forming routes. The green bodies were then sintered using both conventional single and two-step sintering approaches. Synthesis: Two different synthesis methods, viz. precipitation and hydrothermal treatment, were used to synthesize fine α-alumina powders from aluminium chloride, ammonia solution and TEAH (Tetraethyl ammonium hydroxide). XRD, TEM and FEG-SEM were used to characterise the powders produced. The presence of commercial α-alumina powder as seed particles did not affect the transformation to α-alumina phase during the hydrothermal treatment at 220˚C in either basic or acidic environments. The results obtained from the precipitation route showed that the combined effect of adding α-alumina seeds and surfactants to the precursor solution could lower the transformation temperature of α-alumina from about 1200˚C for unseeded samples to 800˚C, as well as reducing the level of agglomeration in the alumina powders. The difference in transformation temperature mainly resulted from the nucleation process by the α-alumina seeds, which enhanced the θ → α transformation kinetics. The lower level of agglomeration present in the final powders could be due to the surface modifying role of the surfactants preventing the particles from growing together during the synthesis process. By introducing a further high-temperature step for a very short duration (1 minute) to the low-temperature heat treatment route (800˚C/12 h), the unseeded sample with added surfactant transformed into pure α-alumina phase. The newly-added step was shown to be an in-situ seeding step, followed by a conventional nucleation and growth process. The best final powder was compared with a commercial α-alumina nanopowder. Processing of alumina ceramics: The effect of low-molecular weight ammonium dispersants including Dispex-A40, Darvan-C and Dolapix-CE64, on high solids content nanoalumina suspensions was investigated. The nanosuspension prepared using the most suitable dispersant, Dolapix-CE64, was slip cast into ~53% dense, very homogeneous green bodies. This nanosuspension was also spray freeze dried into crushable granules using Freon as a foaming agent. Green compacts with density of ~53.5% were then formed by dry pressing the 2 vol% Freon-added spray freeze dried granules at 40 MPa. Both slip cast and die pressed green bodies were sintered using conventional single-step and two-step routes followed by characterising the density and grain size measurement of final dense compacts. The results have been compared with that of a submicron alumina ceramic prepared using a commercial α-alumina suspension. Highly dense alumina with an average grain size of ~0.6 μm was fabricated by means of spark plasma sintering at 1200˚C. The application of 500 MPa allowed achieving almost fully dense alumina at temperature as low as 1200˚C for 30 minutes with no significant grain growth.
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