With the technological development in biologically orientated industries more and more natural products in powdered form are being handled and processed. Three differently comminuted liquorice rhizome products were classified into 23 narrow size fractions to investigate the particle and bulk characteristics of the material, and to study the influence of particle shape on powder flowability. The morphology of the fibrous particulate was investigated by using a Quantimet 720 Image Analyser. The perimeter (P), projected area (A), breadth (B), length (L), horizontal and vertical projected lengths (P V and Pi) and the horizontal and vertical Feret diameters (FV FH) were measured from which four dimensionless shape factors were evaluated, [P2/47rA, PHxPV/A, L/B, FV/FH]. The surface texture of the particles was measured by fractal analysis. The influence of particle shape and size on the mean flow rate, coefficient of flow variation and flow uniformity were measured using a specially designed inclined tube flowmeter. The failure properties of powdered liquorice when sheared under known normal compressive stresses were measured and from a series of yield loci the unconfined yield strength, major consolidation stress and effective angle of internal friction were obtained. The effects of particle shape and size on the angle of internal friction, wall friction, bulk and packed densities were. investigated and the experimental correlations expressed in terms of mathematical equations. These relationships, together with the failure function plots, indicate that comminuted liquorice powder behaves as a "simple" powder.

Master of Science / Food Science Institute / Jayendra K. Amamcharla / Milk protein concentrate (MPC) powders are high-protein dairy ingredients obtained from membrane filtration processes and subsequent spray drying. MPC powders have extensive applications due to their nutritional, functional, and sensory properties. However, their flow properties, rehydration behavior, and morphological characteristics are affected by various factors such as processing, storage, particle size, and composition of the powder. Literature has shown that knowledge about the powder flowability characteristics is critical in their handling, processing, and subsequent storage. For this study, FT4 powder rheometer (FT4, Freeman Technologies, UK) was used to characterize the flowability of MPC powders during storage. This study investigated the flowability and morphological characteristics of commercial MPC powders with three different protein contents (70, 80, and 90%, w/w) after storage at 25ºC and 40ºC for 12 weeks. Powder flow properties (basic flowability energy (BFE), flow rate index (FRI), permeability, etc.) and shear properties (cohesion, flow function, etc.) were evaluated. After 12 weeks of storage at 40ºC, the BFE and FRI values significantly increased (P < 0.05) as the protein content increased from 70 to 90% (w/w). Dynamic flow tests indicated that MPC powders with high protein contents displayed higher permeability. Shear tests confirmed that samples stored at 40ºC were relatively less flowable than samples stored at 25ºC. Also, the lower protein content samples showed better shear flow behavior. The results indicated that MPC powders stored at 40ºC had more cohesiveness and poor flow characteristics than MPC powders stored at 25ºC. The circle equivalent diameter, circularity, and elongation of MPC powders increased as protein content and storage temperature increased, while the convexity decreased as protein content and storage temperature increased. Overall, the MPC powders evidently showed different flow properties and morphological characteristics due to their difference in composition and storage temperature. Literature has shown various methods for determining the solubility of dairy powders, but it requires expensive instruments and skilled technicians. The front-face fluorescence spectroscopy (FFFS) coupled with chemometrics could be used as an efficient alternative, which is commonly used as fingerprints of the various food products. To evaluate FFFS as a useful tool for the non-destructive measurement of solubility in the MPC powders, commercially procured MPC powders were stored at two temperatures (25 and 40ºC) for 1, 2, 4, 8, and 12 weeks to produce powders with different rehydration properties, which subsequently influenced their fluorescence spectra. The spectra of tryptophan and Maillard products were recorded and analyzed with principal components analysis. The solubility index and the relative dissolution index (RDI) obtained from focused beam reflectance measurement was used to predict solubility and dissolution changes using fluorescence spectra of tryptophan and Maillard products. The solubility index and RDI showed that the MPC powders had decreased solubility as the storage time and temperature increased. The results suggest that FFFS has the potential to provide rapid, nondestructive, and accurate measurements of rehydration behavior in MPC powders. Overall, the results indicated that solubility and dissolution behavior of MPC powders were related to protein content and storage conditions that could be measured using FFFS.

Ce travail a pour objectifs d’évaluer le potentiel d'une technique spécifique de caractérisation des propriétés d'écoulement des poudres : le rhéomètre à poudre FT4. L'objectif est de pouvoir mettre en place une analyse complète sur les avantages, les inconvénients et les limites d'utilisation des tests, l'impact de la cohésion des poudres et la répétabilité des mesures. Tout d'abord, des efforts sont faits pour explorer les différences entre la consolidation test de FT4 et le tap-tap. Les résultats indiquent que la consolidation test de FT4 a une bonne répétabilité, mais il peut sous-estimer la compressibilité des poudres. Cette méthode peut être optimisée en améliorant sa procédure d'initialisation pour donner des résultats cohérents en tant que le tap-tap. Deuxièmement, le cisaillement test de FT4 est comparé avec Schulze Ring Shear Tester et Evolution Powder Tester. Cette comparaison indique que le cisaillement test de FT4 peut sous-estimer la cohésion des poudres. Par conséquent, les dimensions des accessoires doivent être optimisées. Enfin, une nouvelle technique de caractérisation a été mise au point. Dans cette méthode, les poudres présentent des mouvements périodiques et la période correspondant peut être liée aux propriétés d'écoulement des poudres. Cette méthode a une très bonne capacité à identifier et à catégorier les propriétés d'écoulement de la poudre dans les conditions de faible contrainte. / This research has been dedicated to evaluate the reliability of the FT4 and to improve the current tests for a better and convenient powder characterization. Firstly, efforts are made to explore the differences between the compaction test provided by the FT4 and the traditional tapped density measurement. Results indicate that the FT4 compaction test has good repetability but it may underestimate powder compressibility. This method can be optimized by improving its initialization procedure to give consistent results as the tapped density measurement. Secondly, the shear tests provided by the FT4 are evaluated by comparing with the methodologies provided by Schulze Ring Shear Tester and Evolution Powder Tester. This comparison indicates that the FT4 shear cell test may underestimate powder strength, especially when a cohesive powder sample is measured, which may cause blockage when using the FT4 method to design a silo. To overcome this shortage, the dimensions of the shear accessories should be optimized. Most importantly, a new characterization technique has been developed. ln this method, powder materials present periodic motions and the cycle time of the periodic flow can be linked to the powder flow properties. This method has very good capability to identify and classify powder flow properties under low stress conditions.

Certains procédés de production d’énergie nécessitent l’utilisation de poudres de biomasse, par exemple la gazéification en réacteur à flux entraîné (RFE). Cependant, les poudres de biomasse ont une mauvaise coulabilité. L’objectif de cette thèse est d’étudier leurs propriétés d’écoulement dans le contexte de la gazéification en RFE, à l’échelle du laboratoire et à l’échelle pilote. A l’échelle du laboratoire, des mesures en tambour rotatif, des tests de cisaillement et des mesures de densité ont été effectués. D’une part, une corrélation est mise en évidence entre la cohésion (issue des tests de cisaillement), la densité et l’angle d’avalanche (tiré des mesures en tambour). Ainsi, un paramètre difficile à obtenir comme la cohésion peut l’être à partir de mesures simples. D’autre part, l’influence de l’humidité sur la coulabilité des poudres de biomasse a été évaluée. L’humidité n’a pas d’effet significatif sous 15 % (en masse, base humide), car l’eau est adsorbée dans la structure de la biomasse ; les particules gonflent et ne sont pas liées par des ponts liquides. Un procédé de granulation humide est proposé. Un liant issu de déchets de biomasse est ajouté à la poudre pour former des granulés d’environ 1 mm. Leur forme sphérique diminue l’entrelacement des particules et leur faible polydispersité diminue le nombre de points de contact. Une amélioration de l’écoulement est observée à l’échelle labo. Une étude énergétique montre que la consommation énergétique du procédé peut descendre jusqu’à 12% du pouvoir calorifique inférieur, ce qui suggère une potentielle rentabilité économique du procédé. Enfin, la caractérisation à l’échelle supérieure est effectuée dans un pilote reproduisant l’injection en RFE. Les résultats montrent le rôle essentiel de la sphéricité et d’une faible polydispersité des particules. L’effet positif de la torréfaction et de la granulation sur la coulabilité est mis en évidence. / Some power generation processes require the biomass to be finely ground, such as biomass gasification in entrained flow reactors. However, fine biomass powders are cohesive and present flow issues. This thesis aims to study the biomass powder flowability in the context of the entrained flow gasification process. Biomass powders are characterized both at laboratory scale and pilot scale. Characterization at lab scale consisted of rotating drum measurements, shear tests and density measurements. First, a correlation is found between the cohesion (derived from shear tests), the powder density and the avalanche angle (derived from the rotating drum measurements). Thus, parameters difficult to get such as the cohesion can be obtained with easy to perform measurements. Then, the influence of moisture content on wood powder flowability has been assessed. No significant effect of the water content is found below 15 wt% (wet basis). Below 15%, as water is adsorbed in the biomass structure, the particles swell without being linked by liquid bridges. A wet granulation method is proposed. Biomass waste binders are added to the powder to form granules around 1 mm. The spherical shape lowers the interlocking phenomenon. The low size dispersity of the grains decreases the number of contact points between particles. An improvement of the flowability at lab scale is observed. An energetic study of the granulation process is proposed, showing the energy consumption can be as low as 12% of the biomass Lowest Heating Value. Thus, the process is potentially economically profitable. Finally, characterization at pilot scale is performed with a device mimicking the injection in an entrained flow reactor. The results show the essential roles in the injection step of both the spherical shape and the narrow size distribution of the particles. The positive effect of torrefaction and granulation on the flowability is highlighted.

With the technological development in biologically orientated industries more and more natural products in powdered form are being handled and processed. Three differently comminuted liquorice rhizome products were classified into 23 narrow size fractions to investigate the particle and bulk characteristics of the material, and to study the influence of particle shape on powder flowability. The morphology of the fibrous particulate was investigated by using a Quantimet 720 Image Analyser. The perimeter (P), projected area (A), breadth (B), length (L), horizontal and vertical projected lengths (P V and Pi) and the horizontal and vertical Feret diameters (FV FH) were measured from which four dimensionless shape factors were evaluated, [P2/47rA, PHxPV/A, L/B, FV/FH]. The surface texture of the particles was measured by fractal analysis. The influence of particle shape and size on the mean flow rate, coefficient of flow variation and flow uniformity were measured using a specially designed inclined tube flowmeter. The failure properties of powdered liquorice when sheared under known normal compressive stresses were measured and from a series of yield loci the unconfined yield strength, major consolidation stress and effective angle of internal friction were obtained. The effects of particle shape and size on the angle of internal friction, wall friction, bulk and packed densities were. investigated and the experimental correlations expressed in terms of mathematical equations. These relationships, together with the failure function plots, indicate that comminuted liquorice powder behaves as a "simple" powder. / Darou-Pakhsh Pharmaceutical Company

No description available.

Additive  manufacturing  technologies  are  widely  used  in  aerospace,  space,  and  turbine industries. Parts can be manufactured directly by selectively adding materials layer-by-layer. A key aspect that is critical to the quality of the final component being manufactured is the powder characteristics. The prevailing powder characterisation techniques help in predicting the flowability of powders but do not relate to the spreading nature of the powder. To create high-quality thin layers of metal powder, it is essential to understand powder spreadability in powder bed-based additive manufacturing processes. The objective of this study was to create spreadability metrics using image analysis, mass analysis, and density analysis. A lab-scale experimental setup was constructed to replicate the powder bed-based additive manufacturing process. The impact of spreading speed and layer thickness on five different steel powders were studied using the suggested metrics. The metrics obtained powder rheometry and revolution powder analysis. The flowability parameters were compared to the spreadability analysis. Image analysis was shown to be efficient to predict the spreading nature of the powder when the processing parameters are varied. One metric, the convex hull ratio, was found to be high for  free-flowing  powders.  The  spread  area  of  free-flowing  powders  was  higher  than  the powders with poor flow properties. A mass-based analysis procedure shows that the ratio of mass deposited to the theoretical mass fluctuated in a systematic manner as a function of testing parameters  and  for  different  powders,  suggesting  that  the  mass  analysis  might  be  another potential   metric   to   assess   spreadability.   The   density-based   analysis   was   effective   in differentiating the layer density of different powders under various experimental conditions. It   is   expected   that   the   proposed   metrics   will   be   a   beginning   for  developing   further characterisation techniques. For example, the layer thickness could be studied by creating a homogenous  layer.  We  anticipate  these  metrics  to  be  used  to  develop  standardisation techniques for defining and quantifying powder spreadability, and thereby improve quality ofadditive manufacturing processes. / Additiv  tillverkning  är  teknologier  som  har  stor  uträckning  inom  flyg-,  rymd  och  turbin industrier. Delar kan bli tillverkade direkt genom att lagervis addera material på varandra. En nyckelaspekt som är kritisk till kvalitén av den slutgiltiga komponenten är egenskaperna hos pulvret. De allmänna teknikerna för pulverkarakterisering hjälper till att förutspå flytförmågan hos pulver men relaterar ej till dess spridningsförmåga. För att kunna skapa högkvalitativa skikt av  metallpulver  är  det  nödvändigt  att  förstå  pulvrets  spridningsförmåga  inom  pulverbädds baserade additiva tillverkningsprocesser. Målet  med denna studie var  att skapa ett mått för spridningsförmågan  genom  bild-  och  massanalys.  Ett  experimentellt  upplägg  i  labbskala konstruerades för att efterlikna en pulverbädds baserad additiv tillverkningsprocess. Effekten av bladets hastighet och lagrets tjocklek på fem olika pulver studerades genom användandet av de  föreslagna  mätetalen.  De  framtagna  mätetalen  jämfördes  sedan  med  existerande  pulver karakteriseringsmetoder  såsom  FT-4  Rheometer  och  pulver  analys  med  hjälp  av  roterande trumma. Slutligen så jämförs flytbarhets parametrarna med spridbarhets mätetalen. Det visar sig att bildanalysen är tillräckligt bra på att förutspå spridningsförmågan hos pulvret när  processparametrarna  låtes  vara  varierande.  Mer  specifikt  så  var  förhållandet  mellan pulvrets yta och det konvexa höljet stort för pulver som visar bra spridning. De framtagna procent  värden  från  massanalysdiagrammen  fluktuerar  vid  olika  processparametrar  hos  de olika  pulvren,  vilket  kan  betyda  att  massanalys  kan  vara  ett  potentiellt  sätt  för  att  mätta spridningsförmågan hos pulver. Det är förväntat att dessa föreslagna mätetal kommer vara början för utveckling av ytterligare karakteriseringstekniker. Till exempel, för att studera densiteten och tjockleken hos ett lager skulle man kunna skapa homogena lager. Vi förutser att dessa mätetal kommer att bli använda för att skapa standardiseringstekniker för att definiera och kvantifiera spridningsförmågan hos ett pulver och genom detta förbättra kvaliteten av den additiva tillverkningsprocessen.

Made available in DSpace on 2016-06-02T19:56:46Z (GMT). No. of bitstreams: 1 4315.pdf: 4002019 bytes, checksum: a7b7282115bf939f257fd8a5748b615e (MD5) Previous issue date: 2012-03-08 / Universidade Federal de Sao Carlos / There are many industries which use powders somewhere in their production process, such as: food, pharmaceuticals, ceramics, cement and fertilizer industries. The knowledge of properties associated with the flowability of these materials is important, since the characteristics of the powders can go through amendments in processing. Thus, the evaluation of indexes of flowability and the identification of main factors which influence the powders flowability play an important role in the operation and design of industrial devices. The objective of this study was to evaluate the flowability properties of organic and inorganic powders, as well as analyze which factors interfered in these properties. The organic materials were represented by whole and skim milk powders, while alumina and ceramic powder were selected for the assessment of inorganic materials. The physical characterizations carried out were: display materials morphology at SEM (Scanning Electron Microscopy), size distribution, particle density, initial moisture content, aerated bulk density and tapped bulk density. The measured materials flowability properties were: angle of internal friction, effective angle of internal friction, angle of wall (galvanized steel) friction and flow index, all of them determined by Jenike's direct shear cell, Hausner ratio obtained from the values of tapped and aerated bulk densities; angle of repose, determined through the dropping of powder in an acrylic surface. In general, the results obtained, considering all methodologies employed for the determination of materials flowability, demonstrated that alumina, ceramic powder and whole milk powder, if compared to skim milk powder, presented lower indexes of flowability. If these materials were stored in silos made of galvanized steel, alumina and ceramic powder flowability would be more difficult than that of skim and whole milk powders. Thus, the results showed that the material physical properties interfere in powders flowability. The skim milk powder flowed more easily than whole milk powder, because higher fat content and smaller average particle size of whole milk powder decreased the flowability of this material in comparison to the skim milk powder. Likewise, despite they have similar composition, alumina presented lower flowability that ceramic powder, because this powder had larger average particle size and the powder presented fewer agglomerated particles. / Existem muitas indústrias que trabalham com pós em alguma parte de seu processo de produção, como: as alimentícias, as farmacêuticas, as cerâmicas, as de cimentos e as de fertilizantes. O conhecimento das propriedades associadas à escoabilidade destes materiais é importante, já que as características dos pós podem sofrer alterações no processamento. Desta forma, a avaliação de índices de escoabilidade e a identificação dos principais fatores que influenciam na escoabilidade de pós são informações que auxiliam as operações industriais e no projeto de equipamentos. Assim, o objetivo deste trabalho foi avaliar a escoabilidade de pós orgânicos e inorgânicos, analisando quais fatores interferiram nesta propriedade. Os materiais escolhidos para representarem os materiais orgânicos foram os leites em pó integral e desnatado, enquanto que a alumina e o pó cerâmico foram selecionados para a avaliação dos materiais inorgânicos. As caracterizações físicas realizadas foram: visualização da morfologia dos materiais no MEV, distribuição granulométrica, massa específica da partícula, teor de umidade inicial, densidade bulk aerada e densidade bulk compactada. A escoabilidade dos materiais foi determinada pelas medidas de: ângulo de atrito interno, ângulo de atrito interno efetivo, ângulo de atrito com a parede de aço galvanizado e índice de escoamento, todos eles determinados pelo cisalhamento direto nas células de Jenike; índice de Hausner obtidos a partir dos valores das densidades bulk compactada e aerada; ângulo de repouso, determinado através do escoamento do pó em uma superfície de acrílico. De maneira geral, os resultados obtidos, considerando-se todas as metodologias empregadas para a determinação da escoabilidade dos materiais, demonstraram que a alumina, o pó cerâmico e o leite em pó integral, se comparados ao leite em pó desnatado, apresentaram menores índices de escoabilidade. Se esses materiais fossem armazenados em silos feitos de aço galvanizado, o escoamento da alumina e do pó cerâmico seria mais difícil do que os leites em pó desnatado e integral. Assim, os resultados mostraram que as propriedades físicas do material interferem na escoabilidade dos pós. O leite em pó desnatado escoou mais facilmente que o leite em pó integral, pois o maior teor de gordura juntamente com o menor tamanho médio das partículas do leite em pó integral diminuíram a escoabilidade deste material em relação ao leite em pó desnatado. Da mesma forma, apesar das composições similares, a alumina apresentou menor escoabilidade que o pó cerâmico, pois este tinha partículas de maior tamanho médio e menos aglomeradas.

Over the past decades, cemented paste backfill (CPB) has become a common, environmentally friendly method of managing mine wastes (such as tailings). This technology allows up to 60% of the total amount of tailings to be reused and filled in the mine stopes after converting them into cemented material. Beside reducing the environmental risks associated with the traditional disposal of these materials, turning them into cemented material and placing them in the underground mine stopes can also provide secondary support for these stopes in addition to minimizing the risk of ground subsidence in the mine area. CPB is an engineered mixture of tailings, water, and hydraulic binder (such as cement, blast furnace slag, and fly ash) that is mixed in the paste plant and delivered into the mine stopes through a gravity or pumping based transportation system. During the transportation of CPB through the delivery system pipelines, the flowability of CPB depends on the rheology of the transported CPB, which is affected by different factors, such as the transportation time, temperature variation, binder type, and chemical composition of these mixtures. In addition, the performance of CPB, after placing the CPB mixture into the mine stopes, is mainly dependent on the role of the hydraulic binder, as it increases the mechanical strength of the mixture through the process of cement hydration. The mechanical strength is also influenced by different factors, such as time progress, temperature variation, and presence of chemical additives. It has previously been found that fresh CPB transported and/or placed in the mine stopes can be susceptible to temperature variation of different sources, such as the climatic effects, heat generated from the surrounding rocks, and heat generated during the process of cement hydration. Unsuitable flowability of CPB through the delivery system might lead to significant financial losses due to clogging of pipelines with unexpected hardening of CPB during transportation, which will cause delay in work and possible damages to the pipelines. Also, failure of CPB structure in the mine stopes due to inappropriate mechanical strength may cause casualties to the mine workers as well as significant environmental and economic damages. Many researchers studied the rheological properties and/or strength development of CPB under the individual effect of any of the aforementioned factors. Additionally, many researchers have evaluated the coupled effect of some of these factors on the rheology and mechanical strength of CPB material. Hitherto, there are currently no studies that addressed the combined effect of all these conditions on the rheological properties and strength development of CPB. At the first stage of this M.A.Sc. study, a series of experimental tests was conducted on fresh CPB in order to determine the combined effect of time, temperature, binder content, and chemical additives on the rheological properties of CPB. These experiments include rheological properties test (yield stress and viscosity), microstructural analysis (thermal analysis and XRD), chemical analysis (pH and Zeta potential), and monitoring tests (electrical conductivity), which were conducted on 125 CPB samples that were mixed and prepared at different temperatures (2oC, 20oC, 35oC) and cured for different curing time (0 hrs., 0.25 hrs., 1 hr., 2hrs, and 4 hrs.). These samples were prepared with different blends of hydraulic binders (PCI, PCI/Slag, and PCI/FA) and contained different dosages of sodium silicate (0%, 0.1%, 0.3%, and 0.5%). The results obtained show that rheology of CPB increases with the progress of curing time. It also increases with the increase in the initial (mixing and curing) temperature and content of sodium silicate. It was also found that the partial usage of slag and FA reduces the rheological properties. However, CPBs containing PCI/FA as binder have lower rheological properties, and thus better flowability, than those that contain PCI/Slag as binder. At the second stage of this M.A.Sc. study, in order to understand the combined effect of time, temperature and sodium silicate content on the strength development of slag-CPB, unconfined compression (UCS) test, microstructural analysis (thermal analysis and MIP), and monitoring tests (electrical conductivity, suction, and volumetric water content) were conducted on 72 CPB samples that were prepared with PCI-Slag as a binder, cured for different times (1 day, 3 days, 7 days, and 28 days) under different curing temperatures of (2oC, 20oC, 35oC), and contained different dosages of sodium silicate (0%, 0.3% and 0.5%). The results obtained at this stage showed that the strength development of slag-CPB increases with the progress of curing time and temperature. It also increases with the increase in the sodium silicate content. Also, the combined effect of high temperature, high dosage of sodium silicate and longer curing time showed significant enhancement in the mechanical strength of slag-CPB. The findings of this M.A.Sc. research will contribute to cost effective, efficient, and safer design of CPB structures in the mine areas. It will also help in minimizing financial loss associated with unsuitable flowability of CPB transported in the CPB delivery system besides reducing the risks of human loss, and the environmental and economic damages associated with the failure of CPB structures.

A preparação de partículas pela técnica de granulação por solidificação de material fundido em leito fluidizado tem se destacado no âmbito da indústria farmacêutica. As vantagens do uso deste método têm atraído muitos pesquisadores para aprimorar e colocar em prática tal técnica de preparo. A principal vantagem deste processo é dispensar o uso de solventes e diminuir o tempo de preparo dos granulados para compressão. O objetivo do presente trabalho foi o desenvolvimento e estudo desta técnica de granulação, usando a lactose tipo spray-dried como substrato e como agente aglutinante uma dispersão do polímero polietilenoglicol 4000 contendo indometacina como fármaco modelo. Outra motivação para este trabalho foi realizar a caracterização físico-química dos granulados obtidos e avaliar um possível aumento da solubilidade deste fármaco de classe II. Resultados obtidos durante estudos preliminares mostram que a solubilidade da indometacina foi consideravelmente aumentada com o uso do PEG e análises físico-química indicaram que não há interação entre a indometacina e o PEG. O método utilizado na granulação consistiu na atomização da dispersão liquefeita de PEG 4000 contendo 25% de indometacina sobre o substrato a fim de obter grânulos contendo estes três componentes. Um estudo prévio da fluidodinâmica da lactose provou ser predominante o regime de leito fluidizado. Para viabilizar a obtenção destas dispersões sólidas, foram estudadas as variáveis do processo como vazão da dispersão carreador/fármaco, vazão do ar de atomização e quantidade total de dispersão adicionada, aplicando para tal um planejamento fatorial tipo Box-Behnken. O leito fluidizado se mostrou eficiente para a granulação e os granulados obtidos foram considerados de boa qualidade baseando-se na sua caracterização por densidades aparente e compactada, fluidez, distribuição granulométrica, doseamento do fármaco e perfil de dissolução in-vitro. Granulados de dois tamanhos médios diferentes e com ótima fluidez foram escolhidos para as análises seguintes. A integridade e ausência de interação do fármaco com os demais componentes destes granulados foram comprovadas por calorimetria exploratória diferencial, difração de raios-X, infravermelho, microscopia de plataforma quente e microscopia de varredura eletrônica. As micrografias mostraram visivelmente que as formas dos cristais de indometacina presentes no granulado apresentaram as características da forma y (II), que é a mesma da indometacina padrão. A dissolução de cápsulas gelatinosas duras contendo os lotes de grânulos escolhidos mostraram que no meio tampão fosfato (pH 7,2) foi liberado até 99% da indometacina. Porém, em meio HCl 0,1N; obteve-se liberação de até 28% da indometacina, o que corresponde a um aumento de 14,5 vezes a liberação obtida com a indometacina padrão. / Recently, there is a renewed interest in the fluidized bed hot melt granulation for the preparation of solid dosage forms in the pharmaceutical industry and academy. The several advantages of this technique have attracted may researchers, but the main advantage are undoubtedly the solvent free operation and the short processing times. The aim of this work was to develop and study this granulation technique using spray-dried lactose as substrate and a dispersion of indomethacin in hot melted polyethylene glycol 4000 and as the binder. Another goal in this work was to characterize the granules obtained and to evaluate any increase in indomethacin solubility in the solid dispersions. The results of preliminary evaluation of indomethacin/polyethylene glycol physical mixtures and solid dispersions showed a considerable increase in the drug solubility, while no chemical or physical interaction with the carrier could be observed. Before the granulation experiments the fluid dynamic behavior of the lactose was characterized as fluidization regime. The method of granulation consisted in the atomization of hot melted polyethylene glycol containing 25% of indomethacin onto the fluidized bed of lactose. In order to study the granulation process, a Box-Behnken design was applied to verify the effects of spray air flow rate, drug/carrier feed rate and total amount of drug/carrier added to granules. The fluidized bed showed to be an effective method for hot melt granulation and the granules quality can be considered adequate, based on their characteristics of apparent and compacted densities, flowability, particle size distribution, indomethacin content and in-vitro dissolution profile. From the whole set of experiments, two granule batches were chosen based on their mean particle sizes and excellent flow indexes, to verify any drug/PEG/lactose interaction during the granulation process. The non existence of interaction was proved by differential scanning calorimetry, X-ray powder diffraction, Fourier transform Infra-red, hot stage microscopy and scanning electron microscopy. The scanning electron microscopy showed that indomethacin crystals with the characteristic shape of the form y (II) could be observed in the granules, indicating that its crystalline form did not change during processing. The dissolution profiles of indomethacin from hard gelatin capsules containing the granules showed the release of 99% of the drug in phosphate buffer media (pH 7.2). However, in acidic media (HCl 0,1N) 28% of the total indomethacin was released, which corresponded to a 14.5 fold increase when compared to the pure indomethacin release under the same conditions.