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Crystal Size Distribution (crystal + size_distribution)
Selected AbstractsUtilization of Focused Beam Reflectance Measurement in the Control of Crystal Size Distribution in a Batch Cooled CrystallizerCHEMICAL ENGINEERING & TECHNOLOGY (CET), Issue 2 2006S. Barthe Abstract Controlling crystal size distribution (CSD) is important to downstream processing and to product quality. The distribution can be characterized by a mean or dominant size and the spread about the mean or dominant size. The development of tools leading to the control of the distribution in a batch crystallizer is the main topic of the present study. An experimentally based control scheme was implemented for batch cooling crystallization of paracetamol from ethanol solutions. Estimates of the CSD in the batch crystallizer were obtained by applying a model of the octahedral paracetamol crystals to a chord length distribution (CLD) obtained from focused beam reflectance measurement (FBRM) and Lasentec software. The model estimates showed reasonably good agreement with results obtained from sieve analyses performed at the end of the runs. [source] Crystallization of Silicate Magmas Deciphered Using Crystal Size DistributionsJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 3 2007Bruce D. Marsh The remoteness and inhospitable nature of natural silicate magma make it exceedingly difficult to study in its natural setting deep beneath volcanoes. Although laboratory experiments involving molten rock are routinely performed, it is the style and nature of crystallization under natural conditions that is important to understand. This is where the crystal size distributions (CSD) method becomes fundamentally valuable. Just as chemical thermodynamics offers a quantitative macroscopic means of investigating chemical processes that occur at the atomic level, crystal size distribution theory quantitatively relates the overall observed spectrum of crystal sizes to both the kinetics of crystallization and the physical processes affecting the population of crystals themselves. Petrography, which is the qualitative study of rock textures, is the oldest, most comprehensively developed, and perhaps most beautiful aspect of studying magmatic rocks. It is the ultimate link to the kinetics of crystallization and the integrated space,time history of evolution of every magma. CSD analysis offers a quantitative inroad to unlocking and quantifying the observed textures of magmatic rocks. Perhaps the most stunning feature of crystal-rich magmatic rocks is that the constituent crystal populations show smooth and often quasi-linear log-normal distributions of negative slope when plotted as population density against crystal size. These patterns are decipherable using CSD theory, and this method has proven uniquely valuable in deciphering the kinetics of crystallization of magma. The CSD method has been largely developed in chemical engineering by Randolph and Larson,1,2 among many others, for use in understanding industrial crystallization processes, and its introduction to natural magmatic systems began in 1988. The CSD approach is particularly valuable in its ease of application to complex systems. It is an aid to classical kinetic theory by being, in its purest form, free of any atomistic assumptions regarding crystal nucleation and growth. Yet the CSD method provides kinetic information valuable to understanding the connection between crystal nucleation and growth and the overall cooling and dynamics of magma. It offers a means of investigating crystallization in dynamic systems, involving both physical and chemical processes, independent of an exact kinetic theory. The CSD method applied to rocks shows a systematic and detailed history of crystal nucleation and growth that forms the foundation of a comprehensive and general model of magma solidification. [source] Influence of citric acid on calcium sulfate dihydrate crystallization in aqueous mediaCRYSTAL RESEARCH AND TECHNOLOGY, Issue 2 2007S. Titiz-Sargut Abstract The crystallization of Calcium sulfate dihydrate produced by the reaction between pure Ca(OH)2 suspension and H2SO4 solution was investigated at different pH values, temperatures and citric acid concentrations. Crystal size distributions, filtration rates and zeta potentials of gypsum were determined as a function of citric acid concentrations at pH 3.5 and 65°C. The influence of citric acid on the morphology of gypsum was also investigated and discussed. The average particle size of gypsum was reached to maximum in the presence of approximately 2500 ppm citric acid concentration, where the minimum cake resistance and maximum filtration rate were obtained. In the presence of citric acid, various crystal morphologies such as tabular, plate-like, double-taper leaf-like and flower-like, etc., were obtained. The change of morphology is related to the preferential adsorption of citric acid on different crystallographic faces. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] A stochastic formulation for the description of the crystal size distribution in antisolvent crystallization processesAICHE JOURNAL, Issue 8 2010M. Grosso Abstract A stochastic approach to describe the crystal size distribution dynamics in antisolvent based crystal growth processes is here introduced. Fluctuations in the process dynamics are taken into account by embedding a deterministic model into a Fokker-Planck equation, which describes the evolution in time of the particle size distribution. The deterministic model used in this application is based on the logistic model, which shows to be adequate to suit the dynamics characteristic of the growth process. Validations against experimental data are presented for the NaCl,water,ethanol antisolvent crystallization system in a bench-scale fed-batch crystallization unit. © 2009 American Institute of Chemical Engineers AIChE J, 2010 [source] Experimental and numerical investigation of the precipitation of barium sulfate in a rotating liquid film reactorAICHE JOURNAL, Issue 8 2009Shengchang Guo Abstract Precipitation of nanosized barium sulfate in a rotating liquid film reactor (RLFR) has been investigated experimentally and through simulations based on the computational fluid dynamics technique including the population balance equation coupled with the Navier,Stokes equations, renormalization group k,, model equations, and species transport equations. A comparative experiment was carried out involving conventional precipitation in a flask. The structure of the precipitate was identified by powder X-ray diffraction (PXRD), which showed that the crystals obtained using the RLFR were smaller in size than those obtained in the flask. Transmission electron microscopy (TEM) images demonstrated that the crystals produced by the two different processes had different morphologies. Further detailed experiments involving varying the operating parameters of the RLFR were performed to investigate the effects on crystal size distribution (CSD). Increasing the speed of the rotor in the RLFR in the range 1000,5000 rpm or increasing the rotor-stator gap in the range 0.1,0.5 mm resulted in a decrease in particle size and narrower particle size distributions. The simulation results suggested that turbulent effects and reaction processes in the effective reactor space were directly related to rotor speed and rotor-stator gap. The simulated volume weighted mean diameter and CSD of particles of barium sulfate were almost identical to the corresponding experimental results obtained using TEM and laser particle size analyzer. The effects of other parameters such as the Kolmogorov scale and competition between induction time and mixing time are also discussed. © 2009 American Institute of Chemical Engineers AIChE J, 2009 [source] Contrasting textural record of two distinct metamorphic events of similar P,T conditions and different durationsJOURNAL OF METAMORPHIC GEOLOGY, Issue 8 2005O. LEXA Abstract A structural, metamorphic and geochronological study of the Staré M,sto belt implies the existence of two distinct metamorphic events of similar peak P,T conditions (700,800 °C, 8,10 kbar) during the Cambro-Ordovician and the Carboniferous tectonometamorphic events. The hypothesis of two distinct periods of metamorphism was suggested on the basis of structural discordance between an undoubtedly Carboniferous granodiorite sill intrusion and earlier Cambro-Ordovician fabrics of a banded amphibolite complex. The analysis of crystal size distribution (CSD) shows high nucleation density (N0) and low average growth rate (Gt) for Carboniferous mylonitic metagabbros and mylonitic granodiorites. The parameter N0 decreases whereas the quantity Gt increases towards higher temperatures progressively approaching the values obtained from the Cambro-Ordovician banded amphibolite complex. The spatial distribution of amphibole and plagioclase shows intense mechanical mixing for lower-temperature mylonitic metagabbros. In high-temperature mylonites a strong aggregate distribution is developed. Cambro-Ordovician amphibolites unaffected by Carboniferous deformation show a regular to anticlustered spatial distribution resulting from heterogeneous nucleation of individual phases. This pattern, together with CSD, was subsequently modified by the grain growth and textural equilibration controlled by diffusive mass transfer during Carboniferous metamorphism. The differences between the observed textures of the amphibolites are interpreted to be a consequence of the different durations of the Carboniferous and Cambro-Ordovician thermal events. [source] Crystal growth rate dispersion modeling using morphological population balanceAICHE JOURNAL, Issue 9 2008Cai Y. Ma Abstract Crystal growth in solution is a surface-controlled process. The variation of growth rates of different crystal faces is considered to be due to the molecular arrangement in the crystal unit cell as well as the crystal surface structures of different faces. As a result, for some crystals, the growth rate for a specific facet is not only a function of supersaturation, but also dependent on some other factors such as its size and the lattice spread angle. This phenomenon of growth rate dispersion (GRD) or fluctuation has been described in literature to have attributed to the formation of some interesting and sophisticated crystal structures observed in experimental studies. In this article, GRD is introduced to a recently proposed morphological population balance model to simulate the dynamic evolution of crystal size distribution in each face direction for the crystallization of potash alum, a chemical that has been reported to show GRD phenomenon and sophisticated crystal structures. The GRD is modeled as a function of the effective relative supersaturation, which is directly related to crystal size, lattice spread angle, relative supersaturation, and solution temperature. The predicted results clearly demonstrated the significant effect of GRD on the shape evolution of the crystals. © 2008 American Institute of Chemical Engineers AIChE J, 2008 [source] Nonlinear kinetic parameter estimation for batch cooling seeded crystallizationAICHE JOURNAL, Issue 8 2004Q. Hu Abstract Kinetic parameter estimation for most batch crystallization processes is necessary because nucleation and crystal growth kinetic parameters are often not available. The existing identification methods are generally based on simplified population balance models such as moment equations, which contain insufficient information on the crystal size distribution (CSD). To deal with these problems, a new optimization-based identification approach for general batch cooling seeded crystallization is proposed in this study. The final-time CSD is directly used for identification. A novel effective method for solving the population balance equation is developed and used to identify nucleation and growth kinetic parameters. Cooling crystallization of ammonium sulfate in water was experimentally investigated, where the concentration was measured by an on-line density meter and the final-time CSD was analyzed by a Malvern Mastersizer 2000. Kinetics for ammonium sulfate are determined based on cooling crystallization experiments. Applying these kinetics in simulation provides a good prediction of the product CSD. © 2004 American Institute of Chemical Engineers AIChE J, 50: 1786,1794, 2004 [source] Fabrication of Structural Leucite Glass,Ceramics from Potassium-Based Geopolymer PrecursorsJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 9 2010Ning Xie Leucite glass,ceramics were fabricated by cold isostatically pressing K2O·Al2O3·4SiO2·11H2O geopolymer powders into pellets followed by firing at 950°,1200°C, every 50°C in air. Leucite formation was observed in specimens heat treated to ,1000°C. The relative density, Vickers hardness, fracture toughness, and biaxial flexural strength of sintered samples ranged approximately 96%,98%, 767,865 kg/mm2, 0.94,2.36 MPa·m1/2, and 90,140 MPa, respectively. The toughness and biaxial flexure strength increased with the firing temperature, while the density and hardness were relatively constant. Scanning electron microscopic and transmission electron microscopic analysis revealed that the sintered geopolymer formed leucite crystals and a compositionally variable glassy phase. Samples heated to 1200°C attained the highest biaxial flexure strength and toughness. This higher strength is believed to arise from an optimum in density, leucite content, and crystal size distribution. [source] Simulation of fine particle formation by precipitation using computational fluid dynamicsTHE CANADIAN JOURNAL OF CHEMICAL ENGINEERING, Issue 5 2000Damien Piton Abstract The 4-environment generalized micromixing (4-EGM) model is applied to describe turbulent mixing and precipitation of barium sulfate in a tubular reactor. The model is implemented in the commercial computational fluid dynamics (CFD) software Fluent. The CFD code is first used to solve for the hydrodynamic fields (velocity, turbulence kinetic energy, turbulent energy dissipation). The species concentrations and moments of the crystal size distribution (CSD) are then computed using user-defined transport equations. CFD simulations are performed for the tubular reactor used in an earlier experimental study of barium sulfate precipitation. The 4-EGM CFD results are shown to compare favourably to CFD results found using the presumed beta PDF model. The latter has previously been shown to yield good agreement with experimental data for the mean crystal size at the outlet of the tubular reactor. On a appliqué un modéle de micromélange généralisé à 4 environnements (4-EGM) afin de décrire le mélange turbulent et la précipitation du sulfate de baryum dans un réacteur tubulaire. Ce modéle a été implanté dans le logiciel de CFD commercial Fluent. Le programme de CFD est d'abord utilisé pour calculer les champs hydrodynamiques (vitesse, énergie cinétique de turbulence, dissipation d'énergie turbulente). Les concentrations d'espéces et les moments de la distribution de taille des cristaux (CSD) sont ensuite calculés par ordinateur à l'aide des équations de transport définies par l'usager. Des simulations de CFD sont réalisées pour le réacteur tubulaire utilisé dans une étude expérimentale antérieure de la précipitation du sulfate de baryum. On montre que les prédictions du 4-EGM se comparent favorablement à celles du modéle béta PDF. II a été montré antérieurement que ce dernier présentait un bon accord avec les donnés expérimentales pour la taille moyenne des cristaux à la sortie du récteur tubulaire. [source] In situ measurement of erythromycin crystal size distribution by focused beam reflective measurement technologyASIA-PACIFIC JOURNAL OF CHEMICAL ENGINEERING, Issue 5 2009Kui Chen Abstract Many factors such as temperature, solvent and water-dosing rate have impact on erythromycin solventing-out process. This article studies the water dosing effect on erythromycin solventing-out process measured by focused beam reflective measurement technology. Our experiments showed that the overall number of nucleated particles went through an explosive increasing after the metastable zone. Followed by a slight decreasing, it reached a relative constancy for a long time. This suggests that earlier crystal nucleation can be induced with higher water dosing rate, nevertheless, it is the same amount of water dosed when the overall crystal number reached its peak during the explosive emergence of crystals. After the overall particle number climaxed, further extension of crystal growth time would not bring any significant increase in crystal size. Copyright © 2009 Curtin University of Technology and John Wiley & Sons, Ltd. [source] Process Optimization of Filling Up CrystallizationCHEMICAL ENGINEERING & TECHNOLOGY (CET), Issue 5 2010I. Markovits Abstract The optimization of filling up crystallization of a specific active pharmaceutical ingredient (APIe) is presented and discussed. Filling up crystallization is a special cooling crystallization method the main goal of which is to narrow the crystal size distribution (CSD) of the product. Fast cooling of the solution is achieved in the first section of the cooling profile as the hot solution of the API for crystallization is fed into the crystallizer, where a constant but significantly lower temperature is maintained by choosing a suitable addition rate of the hot solution and utilizing the cooling efficiency of the crystallizer. The process of determination for formulation of the crystals occurs during the filling up period of the crystallization. As a result of optimization, a parameter range is specified from which the process parameters can be chosen ensuring that the product specifications comply with the limitations. [source] Utilization of Focused Beam Reflectance Measurement in the Control of Crystal Size Distribution in a Batch Cooled CrystallizerCHEMICAL ENGINEERING & TECHNOLOGY (CET), Issue 2 2006S. Barthe Abstract Controlling crystal size distribution (CSD) is important to downstream processing and to product quality. The distribution can be characterized by a mean or dominant size and the spread about the mean or dominant size. The development of tools leading to the control of the distribution in a batch crystallizer is the main topic of the present study. An experimentally based control scheme was implemented for batch cooling crystallization of paracetamol from ethanol solutions. Estimates of the CSD in the batch crystallizer were obtained by applying a model of the octahedral paracetamol crystals to a chord length distribution (CLD) obtained from focused beam reflectance measurement (FBRM) and Lasentec software. The model estimates showed reasonably good agreement with results obtained from sieve analyses performed at the end of the runs. [source] Barium Sulfate Crystallization Kinetics in the Used Quenching Salts Treatment ProcessCHEMICAL ENGINEERING & TECHNOLOGY (CET), Issue 5 2004A. Matynia Abstract The research results and kinetic studies on the barium ions precipitation process by means of crystalline ammonium sulfate addition are presented. The influence of: barium, sodium, potassium and calcium chlorides concentration in the feeding solution and also the process temperature on barium sulfate mass crystallization kinetics are investigated. Experiments were carried out in the MSMPR crystallizer with internal circulation of suspension. The barium sulfate nucleation and crystal growth rates were estimated from crystal size distribution taking into account a size dependent growth (SDG). Research results may be utilized in the used quenching salts processing technology. [source] Modeling Growth Rate Dispersion in Industrial CrystallizersCHEMICAL ENGINEERING & TECHNOLOGY (CET), Issue 3 2003G.M. Westhoff Abstract The phenomenon of healing appears to be a plausible explanation for the growth rate dispersion observed in many industrial crystallizers. In this paper a growth model is postulated, which describes the healing of plastically deformed attrition fragments. The rate of healing is assumed to be inversely proportional to the initial strain and to the rate of change of either the length, the area, or the volume of the crystal. The validity of the proposed model is verified by the simulation of growth of the smallest crystals (L0) in time in a growth experiment for specific combinations of the model parameters. In addition, the applicability of the proposed model is evaluated through simulations of steady state experimental data obtained in a 75-liter Draft Tube (DT) crystallizer. It is concluded that the proposed model is able to fit reasonably well the experimental crystal size distribution. The model predicts the existence of a ,dead time' during which attrition fragments with large initial strain do not grow and which may last several residence times. [source] Modeling the crystallization of proteins and small organic molecules in nanoliter dropsAICHE JOURNAL, Issue 1 2010Richard D. Dombrowski Abstract Drop-based crystallization techniques are used to achieve a high degree of control over crystallization conditions in order to grow high-quality protein crystals for X-ray diffraction or to produce organic crystals with well-controlled size distributions. Simultaneous crystal growth and stochastic nucleation makes it difficult to predict the number and size of crystals that will be produced in a drop-based crystallization process. A mathematical model of crystallization in drops is developed using a Monte Carlo method. The model incorporates key phenomena in drop-based crystallization, including stochastic primary nucleation and growth rate dispersion (GRD) and can predict distributions of the number of crystals per drop and full crystal size distributions (CSD). Key dimensionless parameters are identified to quickly screen for crystallization conditions that are expected to yield a high fraction of drops containing one crystal and a narrow CSD. Using literature correlations for the solubilities, growth, and nucleation rates of lactose and lysozyme, the model is able to predict the experimentally observed crystallization behavior over a wide range of conditions. Model-based strategies for use in the design and optimization of a drop-based crystallization process for producing crystals of well-controlled CSD are identified. © 2009 American Institute of Chemical Engineers AIChE J, 2010 [source] Reaction-induced nucleation and growth v. grain coarsening in contact metamorphic, impure carbonatesJOURNAL OF METAMORPHIC GEOLOGY, Issue 8 2010A. BERGER Abstract The understanding of the evolution of microstructures in a metamorphic rock requires insights into the nucleation and growth history of individual grains, as well as the coarsening processes of the entire aggregate. These two processes are compared in impure carbonates from the contact metamorphic aureole of the Adamello pluton (N-Italy). As a function of increasing distance from the pluton contact, the investigated samples have peak metamorphic temperatures ranging from the stability field of diopside/tremolite down to diagenetic conditions. All samples consist of calcite as the dominant matrix phase, but additionally contain variable amounts of other minerals, the so-called second phases. These second phases are mostly silicate minerals and can be described in a KCMASHC system (K2O, CaO, MgO, Al2O3, SiO2, H2O, CO2), but with variable K/Mg ratios. The modelled and observed metamorphic evolution of these samples are combined with the quantification of the microstructures, i.e. mean grain sizes and crystal size distributions. Growth of the matrix phase and second phases strongly depends on each other owing to coupled grain coarsening. The matrix phase is controlled by the interparticle distances between the second phases, while the second phases need the matrix grain boundary network for mass transfer processes during both grain coarsening and mineral reactions. Interestingly, similar final mean grain sizes of primary second phase and second phases newly formed by nucleation are observed, although the latter formed later but at higher temperatures. Moreover, different kinetic processes, attributed to different driving forces for growth of the newly nucleated grains in comparison with coarsening processes of the pre-existing phases, must have been involved. Chemically induced driving forces of grain growth during reactions are orders of magnitudes larger compared to surface energy, allowing new reaction products subjected to fast growth rates to attain similar grain sizes as phases which underwent long-term grain coarsening. In contrast, observed variations in grain size of the same mineral in samples with a similar T,t history indicate that transport properties depend not only on the growth and coarsening kinetics of the second phases but also on the microstructure of the dominant matrix phase during coupled grain coarsening. Resulting microstructural phenomena such as overgrowth and therefore preservation of former stable minerals by the matrix phase may provide new constraints on the temporal variation of microstructures and provide a unique source for the interpretation of the evolution of metamorphic microstructures. [source] Crystallization of Silicate Magmas Deciphered Using Crystal Size DistributionsJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 3 2007Bruce D. Marsh The remoteness and inhospitable nature of natural silicate magma make it exceedingly difficult to study in its natural setting deep beneath volcanoes. Although laboratory experiments involving molten rock are routinely performed, it is the style and nature of crystallization under natural conditions that is important to understand. This is where the crystal size distributions (CSD) method becomes fundamentally valuable. Just as chemical thermodynamics offers a quantitative macroscopic means of investigating chemical processes that occur at the atomic level, crystal size distribution theory quantitatively relates the overall observed spectrum of crystal sizes to both the kinetics of crystallization and the physical processes affecting the population of crystals themselves. Petrography, which is the qualitative study of rock textures, is the oldest, most comprehensively developed, and perhaps most beautiful aspect of studying magmatic rocks. It is the ultimate link to the kinetics of crystallization and the integrated space,time history of evolution of every magma. CSD analysis offers a quantitative inroad to unlocking and quantifying the observed textures of magmatic rocks. Perhaps the most stunning feature of crystal-rich magmatic rocks is that the constituent crystal populations show smooth and often quasi-linear log-normal distributions of negative slope when plotted as population density against crystal size. These patterns are decipherable using CSD theory, and this method has proven uniquely valuable in deciphering the kinetics of crystallization of magma. The CSD method has been largely developed in chemical engineering by Randolph and Larson,1,2 among many others, for use in understanding industrial crystallization processes, and its introduction to natural magmatic systems began in 1988. The CSD approach is particularly valuable in its ease of application to complex systems. It is an aid to classical kinetic theory by being, in its purest form, free of any atomistic assumptions regarding crystal nucleation and growth. Yet the CSD method provides kinetic information valuable to understanding the connection between crystal nucleation and growth and the overall cooling and dynamics of magma. It offers a means of investigating crystallization in dynamic systems, involving both physical and chemical processes, independent of an exact kinetic theory. The CSD method applied to rocks shows a systematic and detailed history of crystal nucleation and growth that forms the foundation of a comprehensive and general model of magma solidification. [source] Gypsum Crystallization in the Presence of Cr3+ and Citric AcidCHEMICAL ENGINEERING & TECHNOLOGY (CET), Issue 5 2010S. T. Sargut Abstract Reactive crystallization of calcium sulfate dihydrate (gypsum) was investigated at pH 3.5 and 65,°C in the presence of citric acid and Cr3+ ions. Concentrations of both additives varied between 0 and 4000,ppm. The combined effect of additives on crystal size distributions, filtration characteristics, and crystal morphology were investigated and discussed. It was found that the effect of citric acid on gypsum morphology was suppressed in the presence of Cr3+ ions. The change of morphology is related to the complex formation between Cr3+ ions and citric acid at high ion concentrations. [source] | ||||||||||