The development and characterization of bipolar electrode (BPE) focusing is described. BPE focusing is an electrokinetic equilibrium technique in which charged analytes are focused and locally enriched on an electric field gradient in the presence of a counter-flow. This electric field gradient is formed at the boundary of an ion depletion zone – the direct result of faradaic reactions occurring at the BPE in the presence of an externally applied electric field. Direct measurement of the electric field strength in the ion depletion region shows that the electric field is enhanced in this region and takes on a gradient shape, confirming the results of numerical simulations. Transient electric field measurements with simultaneous monitoring of a focused fluorescent tracer reveal that the field gradient forms rapidly upon application of the external field and remains stable over time with the tracer focused at a local field strength predicted by simple electrokinetic equations. These transient electric field measurements probe the effect of individual experimental parameters on the electric field gradient and the focused band. The results of these studies indicate that a steeper field gradient leads to enhanced concentration enrichment of the analyte. The slope of the gradient is increased with higher concentration of the running buffer and higher applied field strength. The addition of pressure driven flow across the microchannel moves the location of the field gradient and the position of the focused band. Further enhancement of enrichment is achieved through the suppression of Taylor dispersion after coating the microchannel with a non-ionic surfactant. The findings of these studies have motivated the transition of BPE focusing to smaller microchannels. A decrease in microchannel size not only decreases Taylor dispersion, but also provides access to higher buffer concentration and higher applied field strength, both of which enhance enrichment. The result is a three-order-of-magnitude increase in total analyte enrichment at a much higher enrichment rate. Furthermore, a dual channel configuration for BPE focusing is introduced which provides greater control over focusing conditions. Finally, the formation of ion depletion and enrichment zones at a BPE in a microchannel is shown to mimic ion concentration polarization (ICP) at micro-/nano-channel junctions. This is significant because this faradaic ICP provides a model to which traditional ICP can be compared and is achieved in a more easily fabricated device. In summary, the fundamental principles of BPE focusing are described. A greater understanding of the effect of experimental parameters on the focusing process leads to an unprecedented magnitude and rate of enrichment in a simple device architecture. / text

No description available.

Submitted by Gustavo Nascimento (gustavo.diniz@ufcg.edu.br) on 2018-02-07T12:18:32Z No. of bitstreams: 1 RAISSA MENEZES DE SOUSA - DISSERTAÇÃO PPGEQ 2016.pdf: 3574277 bytes, checksum: fc3f9b72fefbf347de741a28f9bed6b6 (MD5) / Made available in DSpace on 2018-02-07T12:18:32Z (GMT). No. of bitstreams: 1 RAISSA MENEZES DE SOUSA - DISSERTAÇÃO PPGEQ 2016.pdf: 3574277 bytes, checksum: fc3f9b72fefbf347de741a28f9bed6b6 (MD5) Previous issue date: 2016 / Capes / Diversas tecnologias tem sido utilizadas para tratamento da água produzida (mistura água/óleo). Os processos de separação por membranas (PSM) apresentam vantagens sobre outros métodos tradicionais de separação, contudo alguns problemas operacionais atrelados aos PSM, como polarização por concentração, fouling e formação da camada gel, causam o decréscimo do fluxo permeado com o tempo. Sob condições onde os efeitos da polarização por concentração são mínimas, o escoamento será afetado pela pressão transmembrana. Assim, foi realizado um estudo da fluidodinâmica de uma mistura água/óleo utilizando membrana cerâmica, com auxílio do software ANSYS CFX® Release 15.0. Foi desenvolvido um modelo matemático com um fluido incompressível escoando em regime turbulento. As equações de momento linear, conservação e transporte de massa foram resolvidas com o auxílio de uma malha estruturada. Os resultados da simulação apresentaram os seguintes resultados: a modelagem matemática previu numericamente o processo de filtração tangencial via membrana cerâmica no tratamento de água produzida; observou-se que em vazões muito baixas há uma maior concentração de óleo próximo a membrana enquanto em vazões elevadas, o óleo fica disperso na mistura, onde há a quebra da camada limite; os efeitos viscosos não apresentam diferenças significativas nos perfis de concentração e velocidade. / Several technologies have been used to treat the water produced (water / oil mixture). Membrane separation processes (PSM) have advantages over other traditional methods of separation, however, some operational problems related to PSM, such as polarization by concentration, fouling and formation of the gel layer, cause a decrease in permeate flow over time. Under conditions where the effects of concentration polarization are minimal, the flow will be affected by transmembrane pressure. Thus, a study of the fluid dynamics of a water / oil mixture using ceramic membrane was carried out with the help of ANSYS CFX® Release 15.0 software. A mathematical model was developed with an incompressible fluid flowing in a turbulent regime. The equations of linear momentum, conservation and mass transport were solved with the aid of a structured mesh. The results of the simulation presented the following results: mathematical modeling numerically predicted the process of tangential filtration via the ceramic membrane in the treatment of produced water; it was observed that in very low flows there is a higher concentration of oil near the membrane while at high flow rates the oil is dispersed in the mixture, where the boundary layer is broken; the viscous effects do not present significant differences in the concentration and velocity profiles.

No description available.

This study was to investigate theory and application of Osmotic Distillation (OD). OD is a new novel membrane separation process used for the concentration of aqueous solutions such as fruit juices without the application of heat. The present work was undertaken to investigate flux limitations focusing on feedside, membrane and stripper side characteristics of OD. Once the limiting areas were identified, further studies were undertaken to determine methods of minimizing those limitations without losing the quality and integrity of the liquid feed. A laboratory scale OD system was used to simulate the industrial process which takes place during the production of grape juice concentrate for the fruit juice industry. Results of a UF pretreatment study showed that the use of UF membranes with pore diameters of 0.1 fÝm or less as a pretreatment for the subsequent OD of grape juice resulted in significant increases in OD flux over that observed for juice not subjected to UF. The study of the physical properties of the feed played an important role in the explanation of the OD process. The increase in OD flux was attributed to a reduction in juice viscosity as the result of the removal of protein and other high molecular weight components. Apart from an increase in OD flux, UF pretreatment of the grape juice proved to be beneficial in other areas of the OD process. HPLC measurements showed that the normal concentration of fermentable sugars in standard 68 oBrix concentrate can be achieved at a lower Brix value in feed subjected to UF pretreatment, further reducing the need to handle highly viscous feeds. UF pretreatment also resulted in an increase in juice surface tension consequently reducing the tendency for membrane wet-out to occur. The study of the deoxygenation of the feed solution shows that the removal of dissolved gases by the pre boiling method and the perstraction with chemical reaction (PCR) method both had a positive affect on OD flux. Pre boiling the brine resulted in an indirect reduction in dissolved oxygen in the feed. Pre boiling both the feed and brine, further increased the flux. Throughout the PCR study, it was evident that stripper side mass transfer of O2 was not limited by flowrate but was limited by higher stripper concentration. However, the latter had an insignificant effect when the sulfite-oxygen reaction was catalysed. The use of a catalyst and increase in temperature gave a significant improvement in overall mass transfer coefficient. Ten types of hydrophobic microporous membranes were tested for their influence on OD flux. While the pore diameter is a considerable factor in mass transport of gases through the membrane, it was also noted that the type of membrane material used had an affect on the overall mass transfer. All top three performing membranes had pore diameters of 0.2 x 10-6 m and were made from polytetrafluoroethylene (PTFE). The choice of brine to use as the stripper was based on criteria that were confirmed by the brine studies performed here. The best performing stripper solutions demonstrating the greatest improvement in OD flux over the most commonly used brines, NaCl, CaCl2 and CH3COOK were aqueous solutions of potassium salts of phosphoric acid, pyrophosphoric acid and blends thereof. These salts agreed with all the required characteristics of a suitable brine, demonstrating high solubility rates, supporting the ability to lower water vapour pressure. The study of the corrosion effects of brine salts confirmed the phosphate salts are superior demonstrating some of the lowest corrosion rates and highest pH.

L'accumulation du soluté à la surface d'une membrane entraîne le phénomène de polarisation de concentration. Ceci est un problème qui affecte tous les systèmes de filtration membranaire car il a pour effet une augmentation de la pression osmotique et par conséquence une réduction substantielle du flux de perméat. Afin de comprendre ce phénomène, nous avons d'abord mené une étude analytique de la filtration tangentielle en solvant pur prenant en compte de l'influence de la pression motrice locale sur le taux de perméation. Lors de cette étude, des solutions analytiques qui augmentent en précision avec l'ordre développé ont ete dérivées. Ensuite nous avons développé une approche analytique qui couple l'hydrodynamique aux transferts de matière pour le cas d'un système de filtration qui opère sous haute pression avec un taux de récupération faible. Dans le but d'intégrer à la fois la dépendance de la pression transmembranaire locale sur le flux de perméat et l'influence de la polarisation de concentration à travers leurs effets osmotiques sur la pression effective, nous avons développé un modèle numérique qui résout l'équation de conservation du soluté couplée aux équations de Navier-Stokes en régime stationnaire dans l'approximation de Prandtl. Nous avons validé cette approche grâce aux solutions analytiques précédemment dérivées. Ensuite, nous avons testé l'influence des principaux paramètres de fonctionnement sur la performance du système et comparé nos résultats avec ceux d'autres modèles numériques. Finalement, la pertinence du modèle a été quantitativement vérifiée grâce à des données tirées des expériences bien documentées en osmose inverse. / Concentration polarization of solute at the membrane surface, because of osmotic pressure effects, is an important phenomenon that can cause substantial reductions in permeation. To understand these phenomena: we first analyze the filtration process for a pure solvent, imposing the influence of the driving pressure on permeation at the membrane. We obtain accurate analytical solutions for the flow fields. We then derive an analytical solution that coupled hydrodynamics to mass transfer for filtration systems working in a situation of High Pressure and Low Recovery. Second, we develop a numerical model that incorporates both physical aspects: the dependency of pressure on permeation and the influence of concentration polarization and their related osmotic effects in the effective pressure at the membrane. For that, the numerical approach solves the solute conservation equation coupled with the Navier-Stokes equations under the steady Prandtl approximation. The solution of the system is performed using a finite difference method of order 2. The validity of this approach is successfully demonstrated with the previous analytical solutions for hydrodynamics, as well as for the coupling with mass transfer. We then test the influence of the main operating parameters (inlet concentration, axial flow rate, operating pressure and membrane permeability) on the performance of the filtration system and compare the results with other numerical models that takes into account concentration polarization phenomenon. Finally, the validity of this model is quantitatively well-proved when using the reported data resulting from reverse osmosis experiments.

Les laboratoires sur puce visent à miniaturiser et à intégrer les fonctions couramment utilisées dans les laboratoires d'analyse afin de cibler des applications en santé avec un impact prometteur sur le diagnostic médical au lit du patient. Les membranes poreuses sont d'un grand intérêt pour la préparation et l'analyse d'échantillon sur puce car elles permettent la séparation par taille/charge de molécules, mais également leur pré-concentration. Parmi les matériaux disponibles pour constituer des membranes poreuses, le silicium poreux présente de nombreux avantages tels que le contrôle précis de la taille des pores et de la porosité, une chimie de surface pratique et des propriétés optiques uniques. Les membranes de silicium poreux sont généralement intégrées dans des puces fluidiques en les montant entre deux couches comportant des micro-canaux, formant ainsi des réseaux fluidiques à trois dimensions, peu pratiques et peu adaptés à l'observation directe par microscopie. Dans ces travaux de thèse, nous avons développé deux méthodes de fabrication de membranes de silicium à pores latéraux qui permettent leur intégration monolithique dans des systèmes microfluidiques planaires. Le premier procédé est fondé sur l'utilisation d'électrodes localement structurées afin de guider la formation de pores de manière horizontale, en combinaison avec des substrats type silicium sur isolant (SOI) pour localiser spatialement la formation de silicium poreux dans la profondeur du canal. La deuxième méthode repose sur le fait que la formation de silicium poreux par anodisation est fortement dépendante du type de dopant et de sa concentration. Bien que nous utilisons encore le même type d'électrodes structurées sur les parois latérales de la membrane pour injecter le courant lors de l'anodisation, le dopage par implantation permet de confiner la membrane, de façon analogue mais à la place de l'oxyde enterré du SOI. Des membranes à pores latéraux ont été fabriquées par ces deux méthodes et leur fonctionnalité a été démontrée en réalisant des expériences de filtrage. En plus de la filtration d'échantillon, les membranes ont été utilisées pour étudier la possibilité d'effectuer de la pré-concentration électrocinétique et de la détection interférométrique. La sélectivité ionique des membranes microporeuse permet la pré-concentration moléculaire avec des facteurs de concentration pouvant atteindre jusqu'à 103 en 10 min en appliquant moins de 9 V. Ces résultats sont comparables à ceux rapportés dans la littérature à l'aide par exemple de nanocanaux avec une consommation d'énergie beaucoup plus faible. Enfin, nous avons pu détecter une variation de l'indice de réfraction du silicium poreux par le décalage du spectre d'interférence lors du chargement de différents liquides injectés dans les membranes. Le travail présenté dans cette thèse constitue la première étape dans la démonstration de l'intérêt du silicium poreux pour la préparation d'échantillon et la biodétection dans des laboratoires sur puce planaires. / Lab on a chip devices aim at integrating functions routinely used in medical laboratories into miniaturized chips to target health care applications with a promising impact foreseen in point-of-care testing. Porous membranes are of great interest for on-chip sample preparation and analysis since they enable size- and charge-based molecule separation, but also molecule pre-concentration by ion concentration polarization. Out of the various materials available to constitute porous membranes, porous silicon offers many advantages, such as tunable pore properties, large porosity, convenient surface chemistry and unique optical properties. Porous silicon membranes are usually integrated into fluidic chips by sandwiching fabricated membranes between two layers bearing inlet and outlet microchannels, resulting in three-dimensional fluidic networks that lack the simplicity of operation and direct observation accessibility of planar microfluidic devices. To tackle this constraint, we have developed two methods for the fabrication of lateral porous silicon membranes and their monolithic integration into planar microfluidics. The first method is based on the use of locally patterned electrodes to guide pore formation horizontally within the membrane in combination with silicon-on-insulator (SOI) substrates to spatially localize the porous silicon within the channel depth. The second method relies on the fact that the formation of porous silicon by anodization is highly dependent on the dopant type and concentration. While we still use electrodes patterned on the membrane sidewalls to inject current for anodization, the doping via implantation enables to confine the membrane analogously to but instead of the SOI buried oxide box. Membranes with lateral pores were successfully fabricated by these two methods and their functionality was demonstrated by conducting filtering experiments. In addition to sample filtration, we have achieved electrokinetic pre-concentration and interferometric sensing using the fabricated membranes. The ion selectivity of the microporous membrane enables to carry out sample pre-concentration by ion concentration polarization with concentration factors that can reach more than 103 in 10 min by applying less than 9 V across the membrane[TL1]. These results are comparable to what has already been reported in the literature using e.g. nanochannels with much lower power consumption. Finally, we were able to detect a change of the porous silicon refractive index through the shift of interference spectrum upon loading different liquids into the membrane. The work presented in this dissertation constitutes the first step in demonstrating the interest of porous silicon for all-in-one sample preparation and biosensing into planar lab on a chip.

[ES] La alta cuenca del río Guadalquivir ubicada en el departamento de Tarija, Bolivia, alberga al municipio de la ciudad capital de Tarija; siendo la zona urbana más poblada del departamento. Durante las últimas décadas el departamento ha tenido grandes ingresos económicos, producto de la explotación hidrocarburífera, trayendo consigo un crecimiento poblacional e inmobiliario desproporcionado; originando un proceso de contaminación y degradación ambiental, producto de actividades antrópicas como la disposición de aguas residuales con poco o nulo proceso de tratamiento, desechos sólidos en las orillas del río, y sobreexplotación de áridos. En consecuencia, varias fuentes de abastecimiento de agua se encuentran paralizadas. Durante los últimos años, la problemática ambiental e hídrica ha sido objeto de un permanente debate, sin encontrar soluciones sostenibles en el corto plazo, ocasionando que la degradación ambiental permanezca activa con altos riesgos para la salud púbica. Siendo necesario conocer el estado actual de los recursos hídricos en la cuenca, se realizaron dos trabajos iniciales; se modeló el balance hídrico de la cuenca para establecer la disponibilidad de agua. Para este proceso se realizó una investigación de apoyo destinada a clasificar y determinar las propiedades de los suelos en la cuenca para lograr una menor incertidumbre en los resultados de la modelación hidrológica. Los resultados determinaron que existe un déficit de agua, principalmente en las épocas de estiaje. Un segundo estudio ha sido destinado a conocer la calidad del agua mediante un monitoreo de las principales fuentes de abastecimiento de agua potable. La investigación a las fuentes primarias de agua en la cuenca de estudio identificó la presencia de metales pesados tóxicos para la salud que exceden los límites permisibles para el agua potable. Se identificó plomo, manganeso y hierro presente en los embalses de San Jacinto y Huacata; mientras que el Pb excede en un 50% de lo establecido en la Normativa, el Mn y el Fe superan hasta 800% la norma actual. El trabajo estudia la ósmosis inversa (OI) para eliminar el Pb, Mn y Fe en distintas concentraciones. La principal contribución de esta investigación es el desarrollo y construcción de un modelo matemático novedoso basado en el modelo de concentración de polarización de Spiegler-Kedem. El modelo ha sido desarrollado utilizando diferentes concentraciones de Pb, Mn y Fe. La selección de las concentraciones se basa en construir un modelo que permita el diseño de instalaciones con alta conversión (>80%). Con ello será posible optimizar el proceso desde el punto de vista de eficiencia energética en futuros trabajos. El modelo incluye, además, un factor de ajuste de temperatura tipo Arrhenius que permite una predicción precisa del rendimiento del proceso. La experimentación se llevó a cabo en una planta piloto de OI utilizando una membrana compuesta de poliamida de configuración en espiral tipo ULP 2540 Marca Keensen de procedencia China. La validación del modelo se ajusta correctamente con un error relativo máximo entre los flujos experimental y teórico de 5,4%, 18% y 7.6% para el Pb, Mn y Fe respectivamente. Entre los principales beneficios del estudio, permite garantizar el rechazo de metales superior al 99%, incluso a bajas presiones, garantizando agua segura a la población de Tarija. Como un aporte final se propone un análisis de las partes interesadas en la cuenca, logrando identificar, clasificar y relacionar los diferentes actores con poder e interés en el proyecto. / [CA] L'alta conca del riu Guadalquivir ubicada en el departament de Tarija, Bolívia, alberga al municipi de la ciutat capital de Tarija; sent la zona urbana més poblada del departament. Durant les últimes dècades el departament ha tingut grans ingressos econòmics, producte de l'explotació hidrocarburífera, comportant un creixement poblacional i immobiliari desproporcionat; originant un procés de contaminació i degradació ambiental, producte d'activitats antròpiques com la disposició d'aigües residuals amb poc o nul procés de tractament, rebutjos sòlids a la vora del riu, i sobreexplotació d'àrids. En conseqüència, unes quantes fonts d'abastiment d'aigua es troben paralitzades. Durant els últims anys, la problemàtica ambiental i hídrica ha sigut objecte d'un permanent debat, sense trobar solucions sostenibles en el curt termini, ocasionant que la degradació ambiental romanga activa amb alts riscos per a la salut púbica. Sent necessari conéixer l'estat actual dels recursos hídrics en la conca, es van realitzar dos treballs inicials; es va modelar el balanç hídric de la conca per a establir la disponibilitat d'aigua. Per a este procés es va realitzar una investigació de suport destinada a classificar i determinar les propietats dels sòls en la conca per a aconseguir una menor incertesa en els resultats de la modelació hidrològica. Els resultats van determinar que hi ha un dèficit d'aigua, principalment en les èpoques d'estiatge. Un segon estudi ha sigut destinat a conéixer la qualitat de l'aigua per mitjà d'un monitoreo de les principals fonts d'abastiment d'aigua potable. La investigació a les fonts primàries d'aigua en la conca d'estudi va identificar la presència de metalls pesants tòxics per a la salut que excedixen els límits permissibles per a l'aigua potable. Es va identificar plom, manganés i ferro present en els embassaments de Sant Jacinto i Huacata; mentres que el Pb excedix en un 50% del que establix la Normativa, el Mn i el Fe superen fins a 800% la norma actual. El treball estudia l'osmosi inversa (OI) per a eliminar el Pb, Mn i Fe en distintes concentracions. La principal contribució d'esta investigació és el desenrotllament i construcció d'un model matemàtic nou basat en el model de concentració de polarització de Spiegler-Kedem. El model ha sigut desenrotllat utilitzant diferents concentracions de Pb, Mn i Fe. La selecció de les concentracions es basa a construir un model que permeta el disseny d'instal·lacions amb alta conversió (>80%). Amb això serà possible optimitzar el procés des del punt de vista d'eficiència energètica en futurs treballs. El model inclou, a més, un factor d'ajust de temperatura tipus Arrhenius que permet una predicció precisa del rendiment del procés. L'experimentació es va dur a terme en una planta pilot de OI utilitzant una membrana composta de poliamida de configuració en espiral tipus ULP 2540 Marca Keensen de procedència Xina. La validació del model s'ajusta correctament amb un error relatiu màxim entre els fluxos experimental i teòric de 5,4%, 18% i 7.6% per al Pb, Mn i Fe respectivament. Entre els principals beneficis de l'estudi, permet garantir el rebuig de metalls superior al 99%, inclús a baixes pressions, garantint aigua segura a la població de Tarija. Com una aportació final es proposa una anàlisi de les parts interessades en la conca, aconseguint identificar, classificar i relacionar els diferents actors de poder i interés en el projecte. / [EN] The upper basin of the Guadalquivir River located in the department of Tarija, Bolivia, houses the municipality of the capital city of Tarija; being the most populated urban area of the department. During the last decades the department has had great economic income, as a result of hydrocarbon exploitation, bringing with it a disproportionate population and real estate growth, originating a process of contamination and environmental degradation, product of anthropic activities such as the disposal of wastewater with little or no treatment process, solid waste on the banks of the river, and overexploitation of aggregates. Consequently, various sources of water supply are paralyzed. In recent years, environmental and water problems have been the subject of permanent debate, without finding sustainable solutions in the short term, causing environmental degradation to remain active with high risks to public health. Being necessary to know the current state of the water resources in the basin, two initial works were carried out; the water balance of the basin was modeled to establish the availability of water. For this process, a support investigation was carried out to classify and determine the properties of the soils in the basin to achieve less uncertainty in the results of the hydrological modeling. The results determined that there is a water deficit, mainly in the dry season. A second study has been designed to determine the quality of the water by monitoring the main sources of drinking water supply. The investigation of the primary water sources in the study basin identified the presence of toxic heavy metals for health that exceed the permissible limits for drinking water. Lead, manganese, and iron present in the San Jacinto and Huacata reservoirs were identified; while Pb exceeds by 50% what is established in the Regulation, Mn and Fe exceed up to 800% the current standard. The work studies reverse osmosis (RO) to eliminate Pb, Mn and Fe in different concentrations. The main contribution of this research is the development and construction of a novel mathematical model based on the Spiegler-Kedem concentration polarization model. The model has been developed using different concentrations of Pb, Mn and Fe. The selection of the concentrations is based on building a model that allows the design of installations with high conversion (>80%). With this it will be possible to optimize the process from the point of view of energy efficiency in future works. The model also includes an Arrhenius-type temperature adjustment factor that allows accurate prediction of process performance. The experimentation was carried out in a RO pilot plant using a ULP 2540 Keensen brand spiral configuration polyamide composite membrane from China. The model validation fits correctly with a maximum relative error between the experimental and theoretical fluxes of 5.4%, 18% and 7.6% for Pb, Mn and Fe respectively. Among the main benefits of the study, it allows to guarantee the rejection of metals higher than 99%, even at low pressures, guaranteeing safe water to the population of Tarija. As a final contribution, an analysis of the interested parties in the basin is proposed, managing to identify, classify and relate the different actors with power and interest in the project. / Villena Martínez, EM. (2022). Elaboración de un modelo matemático que permita el análisis de la eficacia de la ósmosis Inversa en el proceso de eliminación de plomo, hierro y manganeso en fuentes de abastecimiento de agua para consumo humano en la cuenca alta del río Guadalquivir en Bolivia y su aporte al crecimiento de la oferta de agua y la disponibilidad sostenible de agua potable a largo plazo [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/191412

A non-reactive model system comprising a highly concentrated and unstable oil-in-water emulsion was used to investigate the retention of oil by the membrane in producing biodiesel with a membrane reactor. Critical flux was identified using the relationship between the permeate flux and transmembrane pressure along with the separation efficiency of the membrane. It was shown that separation efficiencies above 99.5% could be obtained at all operating conditions up to the critical flux. It was observed that the concentration of oil in all collected permeate samples using the oil-water system was below 0.2 wt% when operating at a flux below the critical flux. Studies to date have been limited to the characterization of low concentrated emulsions below 15 vol.%. The average oil droplet size in highly concentrated emulsions was measured as 3200 nm employing direct light scattering (DLS) measurement methods. It was observed that the estimated cake layer thickness of 20 to 80 mm was larger than external diameter of the membrane tube i.e. 6 mm based on a large particle size. Settling of the concentrated emulsion permitted the detection of a smaller particle size distribution (30-100 nm) within the larger particles averaging 3200 nm. It was identified that DLS methods could not efficiently give the droplet size distribution of the oil in the emulsion since large particles interfered with the detection of smaller particles. The content of the smaller particles represented 1% of the total weight of oil at 30°C and 5% at 70°C. This was too low to be detected using DLS measurements but was sufficient to affect ultrafiltration. In order to study the critical flux in the presence of transesterification reaction and the effect of cross flow velocity on separation, various oils were transesterified in another membrane reactor providing higher cross flow velocity. higher cross flow velocity provides better separation by reducing materials deposition on the surface of the membrane due to higher shearing. The oils tested were canola, corn, sunflower and unrefined soy oils (Free Fatty Acids (FFA< 1%)), and waste cooking oil (FFA= 9%). The quality of all biodiesel samples was studied in terms of glycerine, mono-glyceride, di-glyceride and tri-glyceride concentrations. The composition of all biodiesel samples were in the range required by ASTM D6751 and EN 14214 standards. A critical flux based on operating pressure in the reactor was reached for waste cooking and pre-treated corn oils. It was identified that the reaction residence time in the reactor was an extremely important design parameter affecting the operating pressure in the reactor. / Natural Sciences and Engineering Research Council of Canada (NSERC)

A non-reactive model system comprising a highly concentrated and unstable oil-in-water emulsion was used to investigate the retention of oil by the membrane in producing biodiesel with a membrane reactor. Critical flux was identified using the relationship between the permeate flux and transmembrane pressure along with the separation efficiency of the membrane. It was shown that separation efficiencies above 99.5% could be obtained at all operating conditions up to the critical flux. It was observed that the concentration of oil in all collected permeate samples using the oil-water system was below 0.2 wt% when operating at a flux below the critical flux. Studies to date have been limited to the characterization of low concentrated emulsions below 15 vol.%. The average oil droplet size in highly concentrated emulsions was measured as 3200 nm employing direct light scattering (DLS) measurement methods. It was observed that the estimated cake layer thickness of 20 to 80 mm was larger than external diameter of the membrane tube i.e. 6 mm based on a large particle size. Settling of the concentrated emulsion permitted the detection of a smaller particle size distribution (30-100 nm) within the larger particles averaging 3200 nm. It was identified that DLS methods could not efficiently give the droplet size distribution of the oil in the emulsion since large particles interfered with the detection of smaller particles. The content of the smaller particles represented 1% of the total weight of oil at 30°C and 5% at 70°C. This was too low to be detected using DLS measurements but was sufficient to affect ultrafiltration. In order to study the critical flux in the presence of transesterification reaction and the effect of cross flow velocity on separation, various oils were transesterified in another membrane reactor providing higher cross flow velocity. higher cross flow velocity provides better separation by reducing materials deposition on the surface of the membrane due to higher shearing. The oils tested were canola, corn, sunflower and unrefined soy oils (Free Fatty Acids (FFA< 1%)), and waste cooking oil (FFA= 9%). The quality of all biodiesel samples was studied in terms of glycerine, mono-glyceride, di-glyceride and tri-glyceride concentrations. The composition of all biodiesel samples were in the range required by ASTM D6751 and EN 14214 standards. A critical flux based on operating pressure in the reactor was reached for waste cooking and pre-treated corn oils. It was identified that the reaction residence time in the reactor was an extremely important design parameter affecting the operating pressure in the reactor. / Natural Sciences and Engineering Research Council of Canada (NSERC)