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Nesta pesquisa teve-se como objetivo estudar as propriedades físicas de polpas de açaí disponíveis comercialmente, tais como: pH, condutividade, viscosidade, tensão superficial e atenuação acústica, em função da temperatura e de particulados presentes na suspensão de açaí. Foram selecionadas quatro marcas comerciais de polpa de açaí originárias da região norte do Brasil. As amostras foram estudadas na forma pura (sem diluição) e diluídas. As análises de tensão superficial foram conduzidas utilizando o tensiômetro da Sensadyne (modelo QC6000) na faixa de temperatura de 15ºC a 60ºC. Observou-se uma variação da tensão superficial entre as marcas estudadas e em todos os casos a polpa de açaí diluída apresentou tensão superficial superior à polpa pura. Para valores de temperatura maiores que 45ºC, a tensão superficial aumentou com a temperatura para duas marcas estudadas. A verificação da atenuação e do tamanho de partículas foi realizada utilizando a técnica de espectroscopia de atenuação acústica com o equipamento APS-100 (Matec Applied Science, Northborough, USA). A polpa diluída apresentou uma menor atenuação com relação à polpa pura. As polpas de açaí, pura e diluída, apresentaram partículas com tamanho inferior a 0,6 µm de diâmetro, sendo que a polpa pura apresentou partículas com diâmetros maiores. Na investigação reológica foram utilizados reômetros rotacionais (Modelo DVIII+) da marca Brookfield com geometrias de cone-placa e cilindros concêntricos na faixa de temperatura de 15ºC a 60ºC. Os reogramas obtidos foram ajustados aos modelos de Ostwald-de-Waale (Lei da Potência) e Herschel-Bulkley, sendo que o melhor ajuste foi obtido com o modelo de Lei da Potência. Todas as amostras estudadas apresentaram comportamento reológico não-Newtoniano, com características de fluidos tixotrópicos. Foi investigado também o comportamento reológico de polpas de açaí tratadas enzimaticamente para posterior processamento por microfiltração tangencial. As enzimas comerciais Pectinex Ultra SP-L, Biopectinase KK Plus e Ultrazym AFPL foram avaliadas separadamente e a respectiva eficiência foi analisada pela redução da viscosidade no reômetro rotacional com a geometria de cone-plana. A enzima comercial Ultrazym foi mais eficiente na redução da viscosidade aparente da polpa de açaí, sendo que as enzimas Pectinex e Biopectinase não apresentaram alteração significativa da viscosidade. A análise da viscosidade aparente dos produtos (permeado e retentado) da microfiltração utilizando membranas cerâmicas comerciais de 0,8 e 0,2 \'mü\'m foi feita utilizando o reômetro rotacional com a geometria de cone-placa, na temperatura de 25ºC. Para o processamento por microfiltração sem tratamento enzimático, o retentado apresentou valores de viscosidade aparente superior ao permeado e à polpa diluída, enquanto que a polpa diluída apresentou viscosidade aparente superior ao permeado. Na microfiltração com tratamento enzimático a polpa diluída apresentou viscosidade aparente inferior ao permeado, comportamento observado para as duas membranas estudadas (0,8 e 0,2 \'mü\'m). Com os resultados obtidos foi possível verificar a grande variação nas propriedades físicas de polpas comerciais de açaí e com isso, a importância de se realizar tais medidas para a otimização de processos como a microfiltração tangencial. / The main objective of this research was the study of physical properties of commercial types of açaí pulp; including pH, electric conductivity, viscosity, surface tension and acoustic attenuation as a function of temperature and particulates of açaí suspension. Four types of açaí pulp from north region of Brazil were selected. The samples were analyzed in pure (undiluted) and diluted form. Surface tension was measured with Sensadyne tensiometer (model QC6000) in the temperature range: 15º to 60º Celsius. In all types of pulp studied the surface tension of diluted sample was higher than pure sample. For temperatures above 45º Celsius surface tension increased for two types of açai pulp studied. Acoustic attenuation and particle size of samples were analyzed with the equipment APS-100 from Matec Applied Science, Northborough, USA. Acoustic attenuation of diluted samples is smaller for pure samples; the açaí pulp (pure and diluted) has particle sizes below 0,6 µm and the particle sizes of the pure samples were larger than the diluted samples. Brookfield/USA rotational rheometers (Model DVIII+) was employed for rheological analysis with two geometries: cone-plate and concentric cylinders in the temperature range: 15º to 60º Celsius. The rheological behavior was adjusted by Ostwald-de-Waale model (or Power-law model) and Herschel-Bulkley model; the Ostwald-de-Waale model showed a better fit. All brands of pulp studied presented non-Newtonian behavior with tixotropic characteristics. It also investigated the rheological behavior of açaí pulp treated enzymatically for later processing by tangential microfiltration. The commercial enzymes: Pectinex Ultra SP-L (Novozymes - Bagsvaerd, Dinamarca), Biopectinase KK Plus (Kerry Bio-Science) and Ultrazym AFPL (Novozymes - Bagsvaerd, Dinamarca), were utilized to reduce viscosity and the effect was evaluated with the cone-plate geometry of the Brookfield/USA rheometer (Model DVIII+). The data shows that the Ultrazym enzyme was the best option for viscosity reduction of açaí pulp, and the other presented no changes in the viscosity. The viscosity of the retentate and permeate from the microfiltration process (membranes with cut-off 0,8 and 0,2 µm) was determined with the cone-plate geometry of the Brookfield/USA rheometer (Model DVIII+) at 25º Celsius. In microfiltration process without enzymatic action, the apparent viscosity of retentate was always higher than the retentate from diluted pulp. With the results we observed the large variation in physical properties of commercial açaí pulp and thus, the importance of carrying out such measures for the optimization of processes such as tangential microfiltration.

Nesta pesquisa teve-se como objetivo estudar as propriedades físicas de polpas de açaí disponíveis comercialmente, tais como: pH, condutividade, viscosidade, tensão superficial e atenuação acústica, em função da temperatura e de particulados presentes na suspensão de açaí. Foram selecionadas quatro marcas comerciais de polpa de açaí originárias da região norte do Brasil. As amostras foram estudadas na forma pura (sem diluição) e diluídas. As análises de tensão superficial foram conduzidas utilizando o tensiômetro da Sensadyne (modelo QC6000) na faixa de temperatura de 15ºC a 60ºC. Observou-se uma variação da tensão superficial entre as marcas estudadas e em todos os casos a polpa de açaí diluída apresentou tensão superficial superior à polpa pura. Para valores de temperatura maiores que 45ºC, a tensão superficial aumentou com a temperatura para duas marcas estudadas. A verificação da atenuação e do tamanho de partículas foi realizada utilizando a técnica de espectroscopia de atenuação acústica com o equipamento APS-100 (Matec Applied Science, Northborough, USA). A polpa diluída apresentou uma menor atenuação com relação à polpa pura. As polpas de açaí, pura e diluída, apresentaram partículas com tamanho inferior a 0,6 µm de diâmetro, sendo que a polpa pura apresentou partículas com diâmetros maiores. Na investigação reológica foram utilizados reômetros rotacionais (Modelo DVIII+) da marca Brookfield com geometrias de cone-placa e cilindros concêntricos na faixa de temperatura de 15ºC a 60ºC. Os reogramas obtidos foram ajustados aos modelos de Ostwald-de-Waale (Lei da Potência) e Herschel-Bulkley, sendo que o melhor ajuste foi obtido com o modelo de Lei da Potência. Todas as amostras estudadas apresentaram comportamento reológico não-Newtoniano, com características de fluidos tixotrópicos. Foi investigado também o comportamento reológico de polpas de açaí tratadas enzimaticamente para posterior processamento por microfiltração tangencial. As enzimas comerciais Pectinex Ultra SP-L, Biopectinase KK Plus e Ultrazym AFPL foram avaliadas separadamente e a respectiva eficiência foi analisada pela redução da viscosidade no reômetro rotacional com a geometria de cone-plana. A enzima comercial Ultrazym foi mais eficiente na redução da viscosidade aparente da polpa de açaí, sendo que as enzimas Pectinex e Biopectinase não apresentaram alteração significativa da viscosidade. A análise da viscosidade aparente dos produtos (permeado e retentado) da microfiltração utilizando membranas cerâmicas comerciais de 0,8 e 0,2 \'mü\'m foi feita utilizando o reômetro rotacional com a geometria de cone-placa, na temperatura de 25ºC. Para o processamento por microfiltração sem tratamento enzimático, o retentado apresentou valores de viscosidade aparente superior ao permeado e à polpa diluída, enquanto que a polpa diluída apresentou viscosidade aparente superior ao permeado. Na microfiltração com tratamento enzimático a polpa diluída apresentou viscosidade aparente inferior ao permeado, comportamento observado para as duas membranas estudadas (0,8 e 0,2 \'mü\'m). Com os resultados obtidos foi possível verificar a grande variação nas propriedades físicas de polpas comerciais de açaí e com isso, a importância de se realizar tais medidas para a otimização de processos como a microfiltração tangencial. / The main objective of this research was the study of physical properties of commercial types of açaí pulp; including pH, electric conductivity, viscosity, surface tension and acoustic attenuation as a function of temperature and particulates of açaí suspension. Four types of açaí pulp from north region of Brazil were selected. The samples were analyzed in pure (undiluted) and diluted form. Surface tension was measured with Sensadyne tensiometer (model QC6000) in the temperature range: 15º to 60º Celsius. In all types of pulp studied the surface tension of diluted sample was higher than pure sample. For temperatures above 45º Celsius surface tension increased for two types of açai pulp studied. Acoustic attenuation and particle size of samples were analyzed with the equipment APS-100 from Matec Applied Science, Northborough, USA. Acoustic attenuation of diluted samples is smaller for pure samples; the açaí pulp (pure and diluted) has particle sizes below 0,6 µm and the particle sizes of the pure samples were larger than the diluted samples. Brookfield/USA rotational rheometers (Model DVIII+) was employed for rheological analysis with two geometries: cone-plate and concentric cylinders in the temperature range: 15º to 60º Celsius. The rheological behavior was adjusted by Ostwald-de-Waale model (or Power-law model) and Herschel-Bulkley model; the Ostwald-de-Waale model showed a better fit. All brands of pulp studied presented non-Newtonian behavior with tixotropic characteristics. It also investigated the rheological behavior of açaí pulp treated enzymatically for later processing by tangential microfiltration. The commercial enzymes: Pectinex Ultra SP-L (Novozymes - Bagsvaerd, Dinamarca), Biopectinase KK Plus (Kerry Bio-Science) and Ultrazym AFPL (Novozymes - Bagsvaerd, Dinamarca), were utilized to reduce viscosity and the effect was evaluated with the cone-plate geometry of the Brookfield/USA rheometer (Model DVIII+). The data shows that the Ultrazym enzyme was the best option for viscosity reduction of açaí pulp, and the other presented no changes in the viscosity. The viscosity of the retentate and permeate from the microfiltration process (membranes with cut-off 0,8 and 0,2 µm) was determined with the cone-plate geometry of the Brookfield/USA rheometer (Model DVIII+) at 25º Celsius. In microfiltration process without enzymatic action, the apparent viscosity of retentate was always higher than the retentate from diluted pulp. With the results we observed the large variation in physical properties of commercial açaí pulp and thus, the importance of carrying out such measures for the optimization of processes such as tangential microfiltration.

Cette thèse est une étude de l'applicabilité des profileurs acoustiques Doppler horizontaux (H-ADCP) pour le suivi des flux d'eau et de matières en suspension (MES) dans les rivières. Plus d'un an de données acquises avec des H-ADCP de 300, 600 et 1200 kHz sur quatre sites, sur le Rhône, l'Isère et la Saône, avec des géométries et des conditions de forçage contrastées sont analysées. Les résultats montrent qu'une profondeur de section limitée peut poser problème en raison de la diffusion d'une partie de l'énergie acoustique par la surface libre. De plus, quand l'intensité rétrodiffusée par les particules est trop faible, les mesures de vitesse sont sous-estimées ou plus dispersées par rapport aux mesures de référence. Des relations de vitesse indice sont toutefois établies en fonction de l'intensité et de la concentration afin de corriger les vitesses. La concentration en MES est déterminée à partir de l'atténuation acoustique qui est importante pour des suspensions concentrées de limons (> ~100 mg/L). Les constantes d'atténuation sont obtenues par calage sur des mesures de turbidité~; elles sont proches des valeurs théoriques calculées pour les distributions granulométriques des particules primaires. Les mesures acoustiques de concentration sont en bon accord avec les mesures de référence et reproduisent finement la dynamique temporelle. En outre, l'évolution de la granulométrie est étudiée à partir des mesures multi-fréquences d'atténuation sous l'hypothèse que les distributions granulométriques sont lognormales. Cette étude montre qu'une fois que les conditions limites pour des mesures fiables sont bien établies, le H-ADCP est un outil performant pour le suivi des flux d'eau et de MES dans les rivières, surtout pendant des périodes de fortes concentrations telles que des crues. / The work investigates the feasibility of using horizontal acoustic Doppler current profilers (H-ADCPs) to monitor fluxes of water and suspended sediment in rivers. Year-long data sets acquired with H-ADCPs operating at 300, 600 and 1200 kHz at four sites with varying geometries and flow forcing conditions on the Rhône, Saône and Isère rivers are analyzed. Findings show that limited depth can pose a problem due to scattering of a fraction of the acoustic energy from the air-water interface. A second problem arises when the backscattered intensity from the suspended sediment is too weak; this leads to underestimation or higher variability of the velocity estimates compared to reference values. Nevertheless, index-velocity relationships are established as a function of concentration and intensity in order to correct the velocity measurements. Concentrations of suspended sediment can be determined from the acoustic attenuation, which is substantial for silt-sized particles at concentrations > ~100 mg/L. Attenuation constants obtained by comparison with turbidity data are in good agreement with the theoretical values calculated for the measured grain size distributions of the primary particles. The acoustic measurements of concentration are in good agreement with reference methods in terms of both amplitude and temporal resolution. Grain size is determined from multi-frequency attenuation data, accounting for lognormal grain size distributions. Our findings show that once the limits of accurate velocity measurements are well established for a given site and instrument, the side-looking ADCP can be a valuable tool for monitoring concentration and changes in grain size throughout high concentration events such as floods.

Der Neutrinofluss der durch die Wechselwirkung hochenergetischer kosmischer Strahlung mit dem kosmischen Mikrowellenhintergrund entsteht, produziert etwa 0.1 Ereignis/km^3 und Jahr. Um in wenigen Jahren eine ausreichende Anzahl an Ereignissen zu selektieren, muss ein Volumen von mindestens 100 km^3 instrumentiert werden. Die groessten aktuell im Bau befindlichen Detektoren, mit einem Volumen bis zu 1 km^3, benutzen optische Sensoren um das Licht zu detektieren, das durch die Neutrinowechselwirkungen produziert wird. Aus Kostengruenden ist es nicht moeglich mit dieser Technologie 100 mal groessere Detektoren zu bauen. Eine Alternative besteht darin, die durch den bei der Neutrinowechselwirkung entstehenden Teilchenschauer hervorgerufenen akustischen Signale und Radiosignale oder deren Kombination nachzuweisen. Eis ist dafuer ein vielversprechenden Medium, weil es die Moeglichkeit bietet alle drei Signal (optisch, akustisch, radio) nachzuweisen. Eine Grundvoraussetzung fuer die Entwicklung eines solchen Detektors ist die Bestimmung der akustischen Eigenschaften des Eises am Suedpol. Das South Pole Acoustic Test Setup (SPATS) wurde mit dem Ziel gebaut, den Rauschuntergrund, die tiefenabhaengige Schallgeschwindigkeit, die Untergrundereignisrate und die Schall-Abklinglaenge zu messen. Der Detektor besteht aus 4 Trossen, bestueckt mit akustischen Sensoren und Transmittern, die in Tiefen zwischen 80 und 500 m im Eis am Suedpol installiert wurden. Zusaetzlich wurde ein Transmitter (Pinger) entwickelt, der in mehreren wassergefuellten Bohrloechern zum Einsatz kam. Nach drei Jahren ist guter Fortschritt bei der Messung aller beschrieben Groessen erzielt worden. Insbesondere haben es der kombinierte Einsatz von SPATS und des Pingers ermoeglicht, die erste in situ Messung der Abklinglaenge zu 312+68-47 m vorzunehmen. In dieser Arbeit werden die Entwicklung der Hardware, die Analyse und die Resultate dieser Messung vorgestellt. / The neutrino flux generated by the interaction of high energy cosmic rays with the cosmic microwave background is predicted to produce about 0.1 event per km^3 per year. The detection of a sufficient number of events in a few years requires to instrument a volume of at least 100 km^3. The biggest detectors nowadays in construction, covering a volume of about 1 km^3, utilize optical sensors to detect the light produced by neutrino interactions; to extend this instrumentation method by the two necessary orders of magnitude is cost-prohibitive. An alternative is to use the radio or the acoustic signal generated by the neutrino-induced particle cascade, or even better, to use both of them in a hybrid detector. Ice is a promising medium since in principle all three signals can be detected simultaneously. The growing optical experiment IceCube, located at the geographic South Pole, could be complemented with radio and acoustic sensors. A pre-requisite to do so is to measure the acoustic properties of South Pole ice. The South Pole Acoustic Test Setup (SPATS) has been designed to measure background noise, sound speed profile, transient events rate and acoustic attenuation length at that location. The system is comprised of four strings of acoustic sensors and transmitters which are installed at depths between 80 and 500 m. In addition, a retrievable transmitter (called pinger) has been developed and used in several water-filled holes. After almost three years of operation, good progress has been achieved for all the goals. In particular, the attenuation length, one of the most important parameters for determining neutrino detection feasibility, and for which only theoretical estimates were available previously, has now been measured in situ with high confidence to be 312+68-47 m. In this work the hardware developed and the analysis performed to achieve this measurement are presented together with the final result.

Le procédé de broyage en voie humide est une opération intéressante permettant la production de particules fines ou de nanoparticules. La caractérisation de la taille des particules est une donnée essentielle pour l'interprétation des données, le contrôle et l'optimisation de ces procédés selon divers aspects. Il y a un manque de connaissances relatif à la caractérisation de la taille de particules en relation avec les procédés de broyage en voie humide. Cette caractérisation est spécifique pour différentes raisons. (i) Les dispersions traitées par broyage contiennent souvent des impuretés et (ou) des additifs. Nous savons assez peu comment les impuretés et les additifs influencent la taille des particules en suspension dans ces procédés. (ii) Lors de procédés de broyage en voie humide, des dispersions de différentes concentrations peuvent être utilisées. Il est important de savoir comment la concentration de la dispersion peut influencer la mesure de la taille des particules lors du procédé. (iii) La modification de la taille moyenne des particules, résultant de leur fragmentation, est rapide. (iv) Le degré de polydispersité dans le produit change au cours du temps. (v) La nature des interactions entre les particules change; avant broyage les particules sont non-colloïdales, elles le deviennent après un certain temps d'opération. De même, il y a un manque de connaissances permettant de comprendre comment la qualité du produit broyé final est affectée lors du broyage. Dans cette étude nous explorons plusieurs aspects de la caractérisation de taille et de la qualité du produit au cours d'un procédé de broyage en voie humide du CaCO3, réalisé à l'aide d'un broyeur à billes agité. La spectroscopie acoustique qui est une technique connue pour ses potentialités en matière de caractérisation de taille de dispersions en ligne, sous des conditions réelles de procédés et sans nécessiter une dilution des échantillons, a été utilisée dans cette étude en complément de la diffusion dynamique de la lumière. Ce travail a montré sous quelles conditions les effets des impuretés et des additifs etc. sur la taille des particules en suspension pouvaient être déterminés par spectroscopie acoustique. De plus, nous avons comparé et analysé les résultats des mesures de taille obtenus avec les deux techniques. Les différences observées ont été analysées. Nous avons montré que la diffusion multiple observée à forte concentration en solide lors des procédés de broyage en voie humide pouvait conduire à une mauvaise interprétation des résultats relatifs à la taille des particules. En outre, la qualité est un concept relatif. Dans ce travail, nous avons adopté une démarche pour mesurer les effets de différents paramètres sur les caractéristiques du produit broyé en se basant sur une définition de la qualité telle que dans la norme ISO 9000 :2005. La démarche a permis de prendre en compte différents paramètres opératoires importants (tels que les conditions de fonctionnement du broyeur, la mesure de la taille des particules et les propriétés du matériau), ainsi que différentes propriétés caractéristiques du produit (comme la taille moyenne des particules, la largeur de la distribution de taille, la stabilité de la dispersion, le taux d'impuretés, l'énergie spécifique apportée au système et l'apparence visuelle du produit). Nous avons montré que nous pouvions établir une relation entre les paramètres opératoires et différentes qualités de produits obtenus par un procédé de broyage en voie humide. / Wet grinding process is an interesting means of producing fine and nano particles. The particle sizing plays an important role in interpretation, control and optimization of various aspects of the wet grinding process. There is a lack of knowledge in understanding different aspects of particle sizing during a wet grinding process. The particle sizing in a wet grinding process is typical in the sense: (i) The dispersions in a wet grinding process, often, involve additives and (or) impurities. It is less known how impurities and additives influence the particle size of the dispersions in the wet grinding process. (ii) In a wet grinding process, dispersions of different concentrations may be used. It is less known how dispersions of different concentration may influence the particle sizing in a wet grinding process. (iii) In a wet grinding process, the change in average particle size of the product is rapid due to relatively fast breakage of the particles. (iv) The degree of poly dispersity in product changes with grinding time. (v) The nature of interaction between particles is non-colloidal before grinding process; this interaction becomes colloidal after a certain grinding time. Similarly, there is a lack of knowledge to understand how quality of final ground product is influenced in a wet grinding process. This study investigates the different aspects of particle sizing and product quality of aqueous dispersions of CaCO3 in a wet grinding process carried out in a stirred media mill. Acoustic attenuation spectroscopy that is known for measuring particle size of dispersions on line, under real process conditions and without diluting the sample has been employed in the study in addition to the technique of dynamic light scattering. The study brings out the conditions in which the effects of impurities and additives etc. on particle size of the dispersions may be determined using acoustic attenuation spectroscopy. Furthermore, the study compares and analyze the particle sizing results obtained though acoustic attenuation spectroscopy and dynamic light scattering. The causes of differences in the results of two techniques have been investigated. We report presence of multiple scattering at high concentration of the dispersions during wet grinding process that result in misleading results of the particles sizes. Quality is an intangible concept. In order to understand how different operating parameters influence product quality, we propose a method based upon the definition of quality as defined in ISO 9000:2005. The method takes into consideration the important operating parameters of wet grinding process (such as the operating condition of the mill, the measurement of particle size and the material) and important product characteristics ( such as average particle size, range of width of particle size distribution, stability of dispersion, degree of impurities, specific energy input and physical appearance). We bring out how a relationship between operating parameters and products of different grades may be established in a wet grinding process.

Detailed information about the oceanic environment is essential for many applications in the field of marine geology, marine biology, coastal engineering, and marine operations. Especially, knowledge of the properties of the sediment body is often required. Acoustic remote sensing techniques have become highly attractive for classifying the sea bottom and for mapping the sediment properties, due to their high coverage capabilities and low costs compared to common sampling methods. In the last decades, a number of different acoustic devices and related techniques for analyzing their signals have evolved. Each sensor has its specific application due to limitations in the frequency range and resolution. In practice, often a single acoustic tool is chosen based on the current application, supported by other non-acoustic data where required. However, different acoustic remote sensing techniques can supplement each other, as shown in this thesis. Even more, a combination of complementary approaches can contribute to the proper understanding of sound propagation, which is essential when using sound for environmental classification purposes. This includes the knowledge of the relation between acoustics and sediment properties, the focus of this thesis. Providing a detailed three dimensional picture of the sea bottom sediments that allows for gaining maximum insight into this relation is aimed at.<p><p><p>Chapters 4 and 5 are adapted from published work, with permission:<p>DOI:10.1121/1.3569718 (link: http://asadl.org/jasa/resource/1/jasman/v129/i5/p2878_s1) and<p>DOI:10.1109/JOE.2010.2066711 (link: http://ieeexplore.ieee.org/xpl/articleDetails.jsp?tp=&arnumber=5618582&queryText%3Dsiemes)<p>In reference to IEEE copyrighted material which is used with permission in this thesis, the IEEE does not endorse any of the Université libre de Bruxelles' products or services.<p> / Doctorat en Sciences de l'ingénieur / info:eu-repo/semantics/nonPublished