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This thesis addresses the calibration and testing of the Oak Ridge Institute for Science and Education's (ORISE) Holdup Measurement System 4 (HMS4) for use in quantifying U-235 holdup contained within the Process Gas Piping (PGP) of the K-25 Building. In addition to the calibration and testing performed the feasibility of measuring U-238 as a surrogate for U-235 quantification was conducted. A Performance Testing and Validation Plan (PTVP) was developed for confirming the calibration of the system and collecting test data to qualify the HMS4 system for the intended application (ORISE 2009). Tests performed were in accordance with the PTVP and the results were documented in the Performance Testing and Validation Report (PTVR). In turn, the results have been examined to verify that the HMS4 system functions properly and can be used to reliably measure the residual U-235 in pipes. Measurement parameters such as the Lower Level of Detection (LLD), the Minimum Detectable Activity (MDA), and the Total Measurement Uncertainty (TMU) have been determined and reported. To support decommissioning activities, a rapid reliable radiation detection system is needed to assess the amount of residual U-235 within the PGP of the K-25 Building in Oak Ridge, Tennessee. The HMS4 system has been selected to make the required measurements. Verification measurements are considered necessary to assess the reliability and adequacy of the PGP characterization results to ensure criticality incredibility. The purpose of this document is to evaluate the characteristics of the HMS4 system regarding its applicability for use on the east side of K-25. Additionally, to define the level of confidence that should be associated with each HMS4 measurement.

Gravity driven trickle flow of a liquid over a fixed bed in the presence of a gaseous phase is widely encountered throughout the process industry. It is one of the most common ways of contacting multi-phase fluids for reaction or mass transfer purposes. The presence of three phases greatly complicates the mathematical modelling of trickle-bed reactors and makes a description from first principles difficult. Trickle flow performance is usually characterized in terms of hydrodynamic parameters. One such parameter is the liquid holdup. The value and morphology (shape or texture) of the holdup influences the catalyst contacting, wetting, mass transfer characteristics and ultimately the performance of the trickle flow unit. This study is limited to the air-water-glass spheres system with no gas flow. It is partitioned into three sections. An investigation into the nature of the residual liquid holdup in beds of spherical particles revealed that the general assumption that all residual liquid is held in the form of pendular rings at particle contact points proves to be untrue. Instead, indication is that 48 % of the residual holdup is present in the form of agglomerated liquid globules in interstices of low local porosity. Theoretical residual liquid holdup models and residual liquid holdup-based mass transfer models should include this phenomenon. In a subsequent section, the influence of the prewetting procedure on the operating holdup is investigated. Three distinct limiting cases are identified: Kan-wetted, Levec-wetted and non-wetted. A volumetric utilization coefficient that describes the extent to which the bed is irrigated is developed. It indicates that large fractions of the bed remain non-irrigated in the Levec- and non-wetted modes. A momentum balance-based model is adopted to predict the Kan-wetted mode holdup. This model was successfully extended to predicting the holdup in the Levec- and non-wetted modes by simple incorporation of the volumetric utilization coefficient. The predictive capability of this model is highly satisfactory, especially in light of it using only the classical Ergun constants and no fitted parameters (AARE = 9.6 %). The differences in the hysteresis behaviour of holdup and pressure drop in the different modes are attributed to differences in the morphology of the operating holdup. The existence of the three limiting prewetted modes is confirmed by residence time distribution (RTD) analysis of the stimulus-response behaviour of the system. This behaviour was quantified using a NaCl tracer and conductivity measurements at both the inlet and outlet of a bench scale bed. The analyses show that: · There are large fractions of the holdup that is inaccessible to the tracer in the Levec-wetted and non-wetted modes. · The mixedness in the three prewetted modes differ appreciably, with the Kan-wetted mode clearly less mixed than the Levec-wetted mode. The RTD analyses also confirm the existence of the three prewetting modes in a porous system (spherical a-alumina), with a large fraction of the holdup being inaccessible to the tracer in the Levec-wetted mode. This study emphasizes the role of the morphology of the various types of liquid holdup on the hydrodynamic performance of a trickle flow unit. It is apparent that aspects of the morphology depend strongly on phenomena like globule formation, hysteresis and flow and prewetting history that have not been adequately recognized to date. The visualization of the various modes of trickle flow is an intellectual platform from which future studies may be directed. / Dissertation (MEng)--University of Pretoria, 2004. / Chemical Engineering / Unrestricted

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Submitted by Cinthia Konichi Paulo (ckonichi@gmail.com) on 2011-10-07T15:12:21Z No. of bitstreams: 1 cinthia konichi_dissertação.pdf: 511777 bytes, checksum: 1c129baf36f0e318ab7c4303b9e4b2ef (MD5) / Approved for entry into archive by Andrea Virginio Machado (andrea.machado@fgv.br) on 2011-10-17T17:51:30Z (GMT) No. of bitstreams: 1 cinthia konichi_dissertação.pdf: 511777 bytes, checksum: 1c129baf36f0e318ab7c4303b9e4b2ef (MD5) / Made available in DSpace on 2011-10-17T17:53:31Z (GMT). No. of bitstreams: 1 cinthia konichi_dissertação.pdf: 511777 bytes, checksum: 1c129baf36f0e318ab7c4303b9e4b2ef (MD5) Previous issue date: 2011-07-12 / In this survey, we presented the general idea and main results from what we understand that are the most important contributions to contractual solutions to the holdup problem literature. The aim of this paper is to push the previous analysis, uniform the notation and provide a snapshot on the most recent literature, as well as bring topics for future inquires on this issue. / Neste trabalho, apresentamos a ideia geral e principais resultados do que entendemos ser as contribuições mais importantes sobre soluções contratuais ao problema de holdup. O objetivo deste trabalho é investigar os trabalhos de fronteira, uniformizar a notação, assim como apresentar ideias para pesquisa futura.

O escoamento bifásico é muito importante para vários ramos industriais. As misturas bifásicas podem escoar em diversas configurações, as quais são chamadas de padrões de escoamento, e que, ao longo dos anos, receberam diversas classificações. Neste trabalho foi estudado o padrão bolhas dispersas em duto anular. Os trabalhos sobre escoamento bifásico em geometria anular são mais escassos, especialmente quando se trata de dutos anulares de grande dimensão. Dentre os modelos existentes para a modelagem do escoamento bifásico, trabalhamos com o modelo de mistura (Drift Flux), pois, apesar das altas velocidades superficiais, o escoamento em bolhas não possui um comportamento homogêneo, já que a fase gasosa ainda escoa na região central e com uma velocidade maior do que a velocidade da mistura. Foi utilizado o modelo de mistura unidimensional para a modelagem do escoamento bifásico água-ar, pois, além de bastante preciso, é de baixo custo computacional e fácil implementação. Neste trabalho empregamos, a princípio, equações elaboradas para dutos circulares, as quais foram adaptadas para a geometria anular fazendo-se uso do conceito de diâmetro hidráulico. As equações foram implementadas no software Mathematica® e as previsões para o holdup e queda de pressão foram comparadas com dados experimentais próprios. O trabalho experimental foi realizado no laboratório de escoamentos multifásicos do Núcleo de Engenharia Térmica e de Fluidos (NETeF) da EESC-USP, o qual conta com uma instalação experimental em estado operacional para a simulação de escoamentos bifásicos vertical e inclinados em duto anular. Foram colhidas medidas de holdup e queda de pressão bifásica. A concordância entre os dados experimentais e as previsões foi muito satisfatória. / Two-phase flow is present in a wide range of industrial processes. Such flows occur in many geometrical configurations known as flow patterns. In this work is presented a study about bubbly flow in annular duct. Works on two-phase flow in large annular geometry are very scarce. Among the existing models for modeling two-phase flow we chose the drift flux model because the bubbly flow does not behave as a homogeneous mixture, despite of the high superficial velocities, since the gas phase flows faster in the core region in comparison with the mixture velocity. The onedimensional drift flux model besides to be accurate is of low computational cost and easy implementation. The goal of this work is to analyze the prediction of holdup and pressure drop in annular ducts of large diameter. The set of equations used was adapted from those of circular ducts by using the hydraulic diameter concept. The equations were implemented in Mathematica software and holdup and pressure drop prediction were compared with experimental data taken in the experimental facility of the Thermal-fluids Engineering Laboratory of EESC-USP. It was collected measure of holdup and pressure drop. The agreement between experimental data and model predictions is encouraging.

A tecnologia de reatores multifásicos é o coração das transformações químicas de todos os processos industriais, concretamente 99% dos reatores trabalham com a presença de uma ou mais fases. A tomografia é uma técnica poderosa capaz de determinar o efeito de parâmetros operacionais e de desenho na distribuição do holdup das fases, visualizando sistemas opacos de uma forma não invasiva. Um tomógrafo computadorizado de fonte única (SSCT) com capacidade de gerar imagens para as distribuições de holdup em sistemas com duas fases dinâmicas foi desenvolvido e validado com sucesso no CTR/IPEN. Algoritmos para reconstrução de imagens analíticos e discretos ou iterativos (estatísticos) foram desenvolvidos e implementados para tais aplicações e depois comparados. O SSCT foi utilizado para determinar as distribuições de porosidades e de holdup dos sólidos para uma coluna de recheio aleatório. Na Washington University em St. Louis, no Laboratório de Engenharia da Reação Química (CREL), um tomógrafo com duas fontes radioativas (DSCT) capaz de gerar imagens da distribuição do holdup das fases para sistemas dinâmicos com três fases móveis foi validado com êxito. Uma nova metodologia para reconstrução de imagens, que garantiu alta precisão na geração das distribuições do holdup em sistemas de grande porte, foi aplicada. O DSCT permitiu avaliar a influência de parâmetros de operação e do desenho de um aerador em um bioreator na escala piloto. O efeito do desenho de um distribuidor de gás líquido e do regime de escoamento foram determinados para um reator monolítico utilizando o DSCT. Os equipamentos e técnicas desenvolvidas neste trabalho podem ser considerados como uma ferramenta efetiva de pesquisa, intensificando estudos experimentais em uma grande gama de sistemas multifásicos através de geração de imagens. Para isto, foram superadas várias limitações comuns a outras técnicas tomográficas existentes utilizadas no estudo de sistemas com duas e três fases dinâmicas, onde os conhecimentos adquiridos nestes estudos poderão melhorar a compreensão básica dos efeitos de desenho e dinâmica em reatores multifásicos. / It is important to recognize that at the heart of chemical transformations in all process and energy industries is multiphase reator technology, as over 99% of reator systems require the presence of more than one phase for proper operation. Tomography is a powerful technique capable of determining the effect of operating and design parameters on the phase holdup distribution by visualization in opaque flow systems in a noninvasive manner. A single source computed tomography (SSCT) system capable of imaging phase holdup distribution in two phases flow was successfully developed and validated at CTR/IPEN. Analytical and discrete (statistical) image reconstruction algorithms were developed and compared between them. SSCT has been applied to characterize the gas holdup and porosity distributions in a random packed column. At the Chemical Reaction Engineering Laboratory (CREL) of Washington University in St Louis, a novel dual source computed tomography (DSCT) system capable of imaging phase holdup distribution in three phases flow was successfully developed and validated. A new image reconstruction methodology was applied for the image reconstruction of the DSCT which enables accurate imaging of the phase holdup distribution in large scale multiphase systems. DSCT has been applied to characterize the effect of operating parameters and sparger design on the liquid flow behavior of a pilot scale anaerobic bioreactor. Performance studies were carried to access the performance of a gas-liquid distributor and liquid flow in a monolithic reactor using the DSCT. The scanners and techniques developed as part of this work provides an effective research tool for expanding experimental research in a wide range of multiphase flow systems via imaging. It has overcome many limitations, common to the various tomography techniques that exist for imaging systems with two and three phase flow. The knowledge gained from these studies improves the fundamental understanding of the effects of design and dynamics of multiphase reactors.

A tecnologia de reatores multifásicos é o coração das transformações químicas de todos os processos industriais, concretamente 99% dos reatores trabalham com a presença de uma ou mais fases. A tomografia é uma técnica poderosa capaz de determinar o efeito de parâmetros operacionais e de desenho na distribuição do holdup das fases, visualizando sistemas opacos de uma forma não invasiva. Um tomógrafo computadorizado de fonte única (SSCT) com capacidade de gerar imagens para as distribuições de holdup em sistemas com duas fases dinâmicas foi desenvolvido e validado com sucesso no CTR/IPEN. Algoritmos para reconstrução de imagens analíticos e discretos ou iterativos (estatísticos) foram desenvolvidos e implementados para tais aplicações e depois comparados. O SSCT foi utilizado para determinar as distribuições de porosidades e de holdup dos sólidos para uma coluna de recheio aleatório. Na Washington University em St. Louis, no Laboratório de Engenharia da Reação Química (CREL), um tomógrafo com duas fontes radioativas (DSCT) capaz de gerar imagens da distribuição do holdup das fases para sistemas dinâmicos com três fases móveis foi validado com êxito. Uma nova metodologia para reconstrução de imagens, que garantiu alta precisão na geração das distribuições do holdup em sistemas de grande porte, foi aplicada. O DSCT permitiu avaliar a influência de parâmetros de operação e do desenho de um aerador em um bioreator na escala piloto. O efeito do desenho de um distribuidor de gás líquido e do regime de escoamento foram determinados para um reator monolítico utilizando o DSCT. Os equipamentos e técnicas desenvolvidas neste trabalho podem ser considerados como uma ferramenta efetiva de pesquisa, intensificando estudos experimentais em uma grande gama de sistemas multifásicos através de geração de imagens. Para isto, foram superadas várias limitações comuns a outras técnicas tomográficas existentes utilizadas no estudo de sistemas com duas e três fases dinâmicas, onde os conhecimentos adquiridos nestes estudos poderão melhorar a compreensão básica dos efeitos de desenho e dinâmica em reatores multifásicos. / It is important to recognize that at the heart of chemical transformations in all process and energy industries is multiphase reator technology, as over 99% of reator systems require the presence of more than one phase for proper operation. Tomography is a powerful technique capable of determining the effect of operating and design parameters on the phase holdup distribution by visualization in opaque flow systems in a noninvasive manner. A single source computed tomography (SSCT) system capable of imaging phase holdup distribution in two phases flow was successfully developed and validated at CTR/IPEN. Analytical and discrete (statistical) image reconstruction algorithms were developed and compared between them. SSCT has been applied to characterize the gas holdup and porosity distributions in a random packed column. At the Chemical Reaction Engineering Laboratory (CREL) of Washington University in St Louis, a novel dual source computed tomography (DSCT) system capable of imaging phase holdup distribution in three phases flow was successfully developed and validated. A new image reconstruction methodology was applied for the image reconstruction of the DSCT which enables accurate imaging of the phase holdup distribution in large scale multiphase systems. DSCT has been applied to characterize the effect of operating parameters and sparger design on the liquid flow behavior of a pilot scale anaerobic bioreactor. Performance studies were carried to access the performance of a gas-liquid distributor and liquid flow in a monolithic reactor using the DSCT. The scanners and techniques developed as part of this work provides an effective research tool for expanding experimental research in a wide range of multiphase flow systems via imaging. It has overcome many limitations, common to the various tomography techniques that exist for imaging systems with two and three phase flow. The knowledge gained from these studies improves the fundamental understanding of the effects of design and dynamics of multiphase reactors.

O escoamento bifásico é muito importante para vários ramos industriais. As misturas bifásicas podem escoar em diversas configurações, as quais são chamadas de padrões de escoamento, e que, ao longo dos anos, receberam diversas classificações. Neste trabalho foi estudado o padrão bolhas dispersas em duto anular. Os trabalhos sobre escoamento bifásico em geometria anular são mais escassos, especialmente quando se trata de dutos anulares de grande dimensão. Dentre os modelos existentes para a modelagem do escoamento bifásico, trabalhamos com o modelo de mistura (Drift Flux), pois, apesar das altas velocidades superficiais, o escoamento em bolhas não possui um comportamento homogêneo, já que a fase gasosa ainda escoa na região central e com uma velocidade maior do que a velocidade da mistura. Foi utilizado o modelo de mistura unidimensional para a modelagem do escoamento bifásico água-ar, pois, além de bastante preciso, é de baixo custo computacional e fácil implementação. Neste trabalho empregamos, a princípio, equações elaboradas para dutos circulares, as quais foram adaptadas para a geometria anular fazendo-se uso do conceito de diâmetro hidráulico. As equações foram implementadas no software Mathematica® e as previsões para o holdup e queda de pressão foram comparadas com dados experimentais próprios. O trabalho experimental foi realizado no laboratório de escoamentos multifásicos do Núcleo de Engenharia Térmica e de Fluidos (NETeF) da EESC-USP, o qual conta com uma instalação experimental em estado operacional para a simulação de escoamentos bifásicos vertical e inclinados em duto anular. Foram colhidas medidas de holdup e queda de pressão bifásica. A concordância entre os dados experimentais e as previsões foi muito satisfatória. / Two-phase flow is present in a wide range of industrial processes. Such flows occur in many geometrical configurations known as flow patterns. In this work is presented a study about bubbly flow in annular duct. Works on two-phase flow in large annular geometry are very scarce. Among the existing models for modeling two-phase flow we chose the drift flux model because the bubbly flow does not behave as a homogeneous mixture, despite of the high superficial velocities, since the gas phase flows faster in the core region in comparison with the mixture velocity. The onedimensional drift flux model besides to be accurate is of low computational cost and easy implementation. The goal of this work is to analyze the prediction of holdup and pressure drop in annular ducts of large diameter. The set of equations used was adapted from those of circular ducts by using the hydraulic diameter concept. The equations were implemented in Mathematica software and holdup and pressure drop prediction were compared with experimental data taken in the experimental facility of the Thermal-fluids Engineering Laboratory of EESC-USP. It was collected measure of holdup and pressure drop. The agreement between experimental data and model predictions is encouraging.

Commercial ebullated bed hydroprocessors, such as the LC-Finer, are used for the production of synthetic crude oil by upgrading bitumen extracted from the Canadian oil sands. The objectives of this thesis were to experimentally determine bubble characteristics at industrially relevant operating conditions for the design and optimization of the reactor’s recycle pan, as well as to investigate the impact of a catalyst density distribution on the reactor’s fluidization behaviour. High gas holdups have been reported for this type of industrial unit. As a result, high gas holdup conditions were required to assess the commercial unit fluid dynamics. Industrial conditions for the bubble characteristics in the reactor freeboard were simulated in a high pressure gas-liquid bubble column operating at 6.5 MPa using nitrogen and a 0.5 wt.% aqueous ethanol solution. Local bubble characteristics, including gas holdups, bubble rise velocities, and chord lengths, were investigated under various operating conditions using a novel monofibre optical probe designed for high gas holdup and elevated pressure. High gas holdups were achieved (up to 60%) and relatively narrow chord length distributions were observed, where 90% of the bubbles diameters were 1.0 mm or less. The energy dissipated through the distributor plate was shown to have a significant impact on the initial bubble size generated and high gas holdups were also achieved at atmospheric pressure by varying the open-surface area of the distributor. As a result, the impact of catalyst density distribution on local fluidization behaviour was investigated at atmospheric pressure using the previously designed high energy dissipation gas-liquid distributor plate and a 0.5 wt.% aqueous ethanol solution. Fresh and spent hydroprocessing catalysts having relatively narrow and wide density distributions were compared. The introduction of gas greatly impacted the fluidized bed dynamic by rendering the bed-freeboard interface diffuse at low superficial liquid velocity. Bed interface fluctuations were significantly reduced at elevated liquid flow rate due to average bubble size reduction caused by high shearing through the gas-liquid distributor plate. Solid holdup was most affected by the density distribution where bed expansion/contraction was dependent of the liquid flow rate due to varying particle-bubble dynamics.