Preface. 1 Complexes in Solutions. 1.1 Structure of Common Solvents. 1.2 Structure of Pure Aqueous Electrolyte Solutions. 1.2.1 Solvation of Electrolyte Ions in Solutions. 1.2.2 Concentrated and Saturated Electrolyte Solutions. 1.2.3 Formation of Aquo and Partially Aquo Complexes. 1.3 Structure of Aqueous Electrolyte Solutions Containing Additives. 1.4 Polyelectrolytes and Surfactants in Solutions. 1.5 Polydentate Ligands and Molecular Additives. 1.6 Crystal-Additive Interactions. References. 2 Three-Dimensional Nucleation and Metastable Zone Width. 2.1 Driving Force for Phase Transition. 2.2 Three-Dimensional Nucleation of Crystals. 2.2.1 Three-Dimensional Nucleation Rate. 2.2.2 Three-Dimensional Heterogeneous Nucleation. 2.3 Metastable Zone Width. 2.4 Nucleation and Transformation of Metastable Phases. 2.4.1 Crystallization of Metastable Phases. 2.4.2 Overall Crystallization. 2.5 Induction Period for Crystallization. 2.6 Effects of Additives. 2.6.1 Solubility. 2.6.2 Three-Dimensional Nucleation Rate. 2.6.3 Metastable Zone Width. References. 3 Kinetics and Mechanism of Crystal Growth: An Overview. 3.1 Crystal Growth as a Kinetic Process. 3.2 Types of Crystal-Medium Interfaces. 3.3 Roughening of Steps and Surfaces. 3.3.1 Thermodynamic Roughening and the Surface Entropy Factor. 3.3.2 Kinetic Roughening. 3.4 Growth Kinetics of Rough Faces. 3.5 Growth Kinetics of Perfect Smooth Faces. 3.6 Growth Kinetics of Imperfect Smooth Faces. 3.6.1 Surface Diffusion and Direct Integration Models. 3.6.2 Bulk Diffusion Models. 3.6.3 Growth by a Group of Cooperating Screw Dislocations. 3.6.4 Preferential Growth at Edge Dislocations. 3.7 Effect of Foreign Substances on Growth Kinetics. 3.7.1 Some General Considerations. 3.7.2 Growth Kinetics by Heterogeneous Two-Dimensional Nucleation. 3.8 Real Crystal Growth Mechanisms. 3.8.1 Structure of Interfacial Layer. 3.8.2 Sources of Growth Steps. 3.9 Techniques for Studying Growth Kinetics. References. 4 Effect of Impurities on Crystal Growth Kinetics. 4.1 Mobile and Immobile Impurities. 4.2 Surface Coverage and Adsorption Isotherms. 4.2.1 Adsorption Isotherms. 4.2.2 Changes in Surface Free Energy by Adsorption of Impurities. 4.3 Kinetic Models of Impurity Adsorption. 4.3.1 Earlier Models. 4.3.2 Velocity of Curved Steps. 4.3.3 Impurity Adsorption at Kinks in Steps: Kubota-Mullin Model. 4.3.4 Impurity Adsorption at Surface Terrace: Cabrera-Vermilyea Model. 4.3.5 Effectiveness Factor for Impurity Adsorption. 4.3.6 Adsorption of Two Competing Impurities. 4.4 Confrontation of Impurity Adsorption Mechanisms with Experimental Data. 4.5 Time-Dependent Impurity Adsorption. 4.6 Growth Kinetics in the Presence of Impurities. 4.6.1 Basic Kinetic Equations. 4.6.2 Time Dependence of Face Displacement. 4.6.3 Dependence of Kinetic Coefficient for Step Motion on Impurity Concentration. 4.7 Tapering of KDP-Type Crystals. 4.8 Growth-Promoting Effects of Impurities. 4.8.1 Decrease in Step Free Energy and Roughening of Steps. 4.8.2 Formation of Surface Macroclusters. 4.9 Impurity Adsorption on Rough Faces. 4.10 Formation of Two-Dimensional Adsorption Layer. 4.11 Interactions Between Additives and Crystal Interface. 4.11.1 Nature of Impurity-Crystal Interactions. 4.11.2 Chemical Aspects of Impurity-Crystal Interactions. 4.12 Tailor-Made Additives. References. 5 Dead Supersaturation Zone and Threshold Supersaturations for Growth. 5.1 Origin of Threshold Supersaturations for Growth. 5.1.1 Basic Kinetic Equations. 5.1.2 Three Different Distances Between Impurity Particles. 5.2 Determination of Threshold Supersaturations from v(sigma) and R(sigma) Data. 5.2.1 Relationship Between the Model Involving Cooperating Spirals and the Power-Law Approach. 5.2.2 Relationship Between the Power-Law Approach and an Empirical Expression with Corrected Supersaturation. 5.2.3 Determination of sigma. 5.3 Dependence of Threshold Supersaturations on Impurity Concentration: Basic Theoretical Equations and Linear Approximations. 5.4 Confrontation of Theoretical Equations with Experimental Data. 5.4.1 Impurity Adsorption at Kinks and Surface Terrace. 5.4.2 Threshold Supersaturations and Impurity Adsorption Isotherms. 5.5 Impurity Adsorption and Solution Supersaturation. 5.6 Dependence of Ratios sigmad/sigma and sigma/sigma on ci References. 6 Mineralization in Natural and Artificial Systems. 6.1 Biomineralization as a Process. 6.1.1 Structure and Composition of Biominerals. 6.1.2 Humans and Animals. 6.1.3 Plants. 6.1.4 Mollusk Shells and Avian Eggshells. 6.2 Pathological Mineralization. 6.3 Effect of Biologically Active Additives on Crystallization Processes. 6.3.1 Overall Precipitation Kinetics. 6.3.2 Overall Growth Kinetics. 6.3.3 Phases and Polymorphs of Crystallizing Calcium Salts. 6.3.4 Transformation of Metastable Phases. 6.4 Scale Formation and Salt Weathering. References. 7 Morphology and Size Distribution of Crystals. 7.1 Growth Morphology of Crystals. 7.1.1 General Concepts. 7.1.2 Effect of Additives on Surface Morphology. 7.1.3 Effect of Solvent on Crystal Morphology. 7.1.4 Growth Morphodroms. 7.2 Ostwald Ripening and Crystal Size Dispersion. 7.3 Crystal Size Distribution. 7.3.1 Population Balance Approach. 7.3.2 Balanced Nucleation-Growth Approach. 7.3.3 Approach Based on Law of Proportionate Effect. 7.3.4 Effect of Additives on Crystal Size Distribution. 7.4 Control of Shape and Size of Particles. 7.4.1 Growth-Directed Synthesis. 7.4.2 Template-Directed Synthesis. 7.5 Biological Tissue Engineering. References. 8 Additives and Crystallization Processes in Industries. 8.1 Pharmaceutical Industry. 8.1.1 Nucleation, Growth and Morphology of Drug Crystals. 8.1.2 Preparation and Size Distribution of Drug Particles. 8.2 Petroleum Industry. 8.2.1 Some Basic Concepts. 8.2.2 Crystallization Behavior of Linear Long-Chain n-Alkanes. 8.2.3 Biodiesels and their Crystallization Behavior. 8.3 Food Industry. 8.3.1 Some Basic Concepts. 8.3.2 Crystallization of Food Fats in the Bulk. 8.3.3 Crystallization of Polymorphs. 8.3.4 Crystallization of Fats and Oils in Emulsion Droplets. 8.3.5 Number of Nucleation Centers and Overall Crystallization in Emulsion Systems. References. 9 Incorporation of Impurities in Crystals. 9.1 Types of Impurity Incorporation and the Segregation Coefficient. 9.2 Equilibrium Segregation Coefficient. 9.2.1 Binary Mixture Approach. 9.2.2 Thermodynamic Approach. 9.2.3 Theoretical Predictions and their Comparison with Experimental Data on Segregation Coefficient. 9.3 Effective Segregation Coefficient. 9.3.1 Volume Diffusion Model. 9.3.2 Diffusional Relaxation Approach. 9.3.3 Statistical Selection Approach. 9.3.4 Surface Adsorption Approach. 9.4 Relationship Between Effective Segregation Coefficient and Face Growth Rate. 9.5 Threshold Supersaturation for Trapping of Impurities During Growth. 9.6 Effective Segregation Coefficient and Internal Stresses Caused by Impurities. References. List of Symbols. Subject Index. Author Index.
Preface. 1. Introduction to Crystallization Issues. 1.1 Crystal Properties and Polymorphism (Chapters 2 and 3). 1.2 Nucleation and Growth Kinetics (Chapter 4). 1.3 Critical Issues (Chapter 5). 1.4 Mixing and Crystallization (Chapter 6). 1.5 Crystallization Process Options (Chapters 7-10). 1.6 Special Applications (Chapter 11). 1.7 Regulatory Issues. 2. Properties. 2.1 Solubility. 2.2 Supersaturation, Metastable Zone, and Induction Time. 2.3 Oil, Amorphous, and Crystalline States. 2.4 Polymorphism. 2.5 Solvate. 2.6 Solid Compound, Solid Solution, and Solid Mixture. 2.7 Inclusion and Occlusion. 2.8 Adsorption, Hygroscopicity, and Deliquescence. 2.9 Crystal Morphology. 2.10 Particle Size Distribution and Surface Area. 3. Polymorphism. 3.1 Phase Rule. 3.2 Phase Transition. 3.3 Examples. Example 3-1 Indomethacin. Example 3-2 Sulindac. Example 3-3 Losartan. Example 3-4 Finasteride. Example 3-5 Ibuprofen Lysinate. Example 3-6 HCl Salt of a Drug Candidate. Example 3-7 Second HCl Salt of a Drug Candidate. Example 3-8 Prednisolone t-Butylacetate. Example 3-9 Phthalylsulfathiazole. 3.4 Future Direction. 4. Kinetics. 4.1 Supersaturation and Rate Processes. 4.2 Nucleation. 4.3 Crystal Growth. 4.4 Nucleate/Seed Aging and Ostwald Ripening. 4.5 Delivered Product: Size Distribution and Morphology. 5. Critical Issues in Crystallization Practice. 5.1 Introduction. 5.2 Nucleation. 5.3 Growth. 5.4 Oiling Out, Agglomeration/Aggregation. 5.5 Seeding. 5.6 Rate of Generation of Supersaturation. 5.7 Summary of Critical Issues. 6. Mixing and Crystallization. 6.1 Introduction. 6.2 Mixing Considerations. 6.3 Mixing Effects on Nucleation. 6.4 Mixing Effects on Crystal Growth. 6.5 Mixing Scale-up. 6.6 Crystallization Equipment. Example 6-1. 7. Cooling Crystallization. 7.1 Batch Operation. 7.2 Continuous Operations. 7.3 Process Design-Examples. Example 7-1 Intermediate in a Multistep Synthesis. Example 7-2 Pure Crystallization of an API. Example 7-3 Crystallization Using the Heel from the Previous Batch as Seed. Example 7-4 Resolution of Ibuprofen Via Stereospecific Crystallization. Example 7-5 Crystallization of Pure Bulk with Polymorphism. Example 7-6 Continuous Separation of Stereoisomers. 8. Evaporative Crystallization. 8.1 Introduction. 8.2 Solubility Diagrams. 8.3 Factors Affecting Nucleation and Growth. 8.4 Scale-up 171 8.5 Equipment. Example 8-1 Crystallization of a Pharmaceutical Intermediate Salt. Example 8-2 Crystallization of the Sodium Salt of a Drug Candidate. 9. Antisolvent Crystallization. 9.1 Semibatch Operation. Example 9-1 Crystallization of an Intermediate. Example 9-2 Rejection of Isomeric Impurities of Final Bulk Active Product. Example 9-3 Crystallization of a Pharmaceutical Product with Poor Nucleation and Growth Characteristics. Example 9-4 Impact of Solvent and Supersaturation on Particle Size and Crystal Form. 9.2 In-Line Mixing Crystallization. Example 9-5 Crystallization of an API Using Impinging Jets. Example 9-6 Crystallization of a Pharmaceutical Product Candidate Using an Impinging Jet with Recycle. 10. Reactive Crystallization. 10.1 Introduction. 10.2 Control of Particle Size. 10.3 Key Issues in Organic Reactive Crystallization. 10.4 Scale-up. Example 10-1 Reactive Crystallization of an API. Example 10-2 Reactive Crystallization of an Intermediate. Example 10-3 Reactive Crystallization of a Sodium Salt of an API. Example 10-4 Reactive Crystallization of an API. 10.5 Creation of Fine Particles-In-Line Reactive Crystallization. 11. Special Applications. 11.1 Introduction. 11.2 Crystallization with Supercritical Fluids. 11.3 Ultrasound in Crystallization. 11.4 Computational Fluid Dynamics in Crystallization. Example 11-1 Sterile Crystallization of Imipenem. Example 11-2 Enhanced Selectivity of a Consecutive-Competitive Reaction by Crystallization of the Desired Product During the Reaction. Example 11-3 Applying Solubility to Improve Reaction Selectivity. Example 11-4 Melt Crystallization of Dimethyl Sulfoxide. Example 11-5 Freeze Crystallization of Imipenem. Example 11-6 Continuous Separation of Stereoisomers. 11.5 Strategic Considerations for Development of a New Crystallization Process. References. Index.
Thermodynamics of Nucleation: First-Order Phase Transitions Driving Force for Nucleation Work for Cluster Formation Nucleus Size and Nucleation Work Nucleation Theorem Properties of Clusters Equilibrium Cluster Size Distribution Density-Functional Approach. Kinetics of Nucleation: Master Equation Transition Frequencies Nucleation Rate Equilibrium Stationary Nucleation First Application of the Nucleation Theorem Nonstationary Nucleation Second Application of the Nucleation Theorem Nucleation at Variable Supersaturation. Factors affecting Nucleation: Seed size Line Energy Strain Energy Electric Field Carrier-Gas Pressure Solution Pressure Preexisting Clusters Active Centres. Applications: Overall Crystallization Crystal Growth Third Application of the Nucleation Theorem Induction Time Fourth Application of the Nucleation Theorem Metastabiltiy Limit Maximum Number of Supernuclei Size Distribution of Supernuclei Growth of Thin Films Lifetime of Amphiphile Bilayers. Appendices References Author index Subject Index.
Preface. Introduction. Physico-Chemical Interaction Between Magnesium and Rare-earth Metals. Decomposition of the Supersaturated Solid Solutions in Mg-RE Alloys. Peculiarities of the Plastic Deformation and Recrystallization in Mg-RE Alloys. Effect or Rare-earth Metals on Mechanical and Some Other Properties of Magnesium. Commercial Magnesium Alloys with Rare-earth Metals, Their Compositions and Properties. Conclusion. References. Subject. Index.
CRYSTALLIZATION: INTRODUCTION MECHANISMS OF CRYSTALLIZATION Crystal Lattice Nucleation of Crystals Growth and Growth Rate of Crystals SOLUBILITY AND SOLUTION EQUILIBRIA IN CRYSTALLIZATION Phase Equilibria and Phase Diagrams: General Issues Melt Phase Diagrams Solution Equilibria AGGLOMERATION DURING CRYSTALLIZATION Mechanisms and Kinetics of Agglomeration Parameters Influencing Agglomeration Agglomeration during Crystallization Mechanical Properties of Agglomerates POLYMORPHISM OF CRYSTALLINE SYSTEMS Introduction and Definitions Occurrence and Properties of Polymorphs and Solvates Thermodynamics of Polymorphs of Solid-State Forms Thermodynamics of Hydrates Experimental Techniques to Elucidate Thermodynamics Formation of Various Polymorphs and Solid-State Forms-Polymorph Screens Selection of Optimal Form for Development THE INFLUENCE OF ADDITIVES AND IMPURITIES ON CRYSTALLIZATION Influence of Additives and Impurities on Crystallization Influence of Impurities: Modeling Tailor-Made Additives Modeling the Influence of Solvents PURIFICATION BY CRYSTALLIZATION Introduction Mechanisms of Impurity Incorporation and Purification CHARACTERIZATION OF CRYSTALLINE PRODUCTS Introduction Characterization of Intrinsic Properties of a Solid Characterization of Particle Shape and Size Powder Flow Properties In-Process Characterization BASICS OF INDUSTRIAL CRYSTALLIZATION FROM SOLUTION Generation of Supersaturation in a Crystallizer Mass and Population Balance for Growth from Suspension Operation of a Continuous Crystallizer: Basics Operation of a Batch Crystallizer: Basics DEVELOPMENT OF BATCH CRYSTALLIZATIONS Setting Goals Crystallization of Organic Moieties Generation of Supersaturation in Batch Crystallizations Initiation of Crystallization - Nucleation Phase Seeded Batch Crystallizations Crystallization Period Scale-Up Considerations Manipulating Particle Shape CONTINUOUS CRYSTALLIZATION Concept and Design of Continuous Crystallizers Various Continuous Crystallizers Periphery Special Features of the Process Adjustment of Suspension Densities PRECIPITATION Precipitation from Solution by Mixing Two Streams Semi-Batch Precipitations Model of Mixing during Precipitation Precipitations Using Supercritical Fluids Crystal Issues Particle Size as a Function of Operating Conditions MIXING IN CRYSTALLIZATION PROCESSES Mixing in Batch and Continuous Crystallization Processes Basic Mixing Tasks - Mixing Tasks in Crystallization Impellers and Agitation Systems Power Consumption of an Impeller System [2] Blending Suspending Scale-Up of a Crystallization Process DOWNSTREAM PROCESSES Transfer of Suspension and Filter Cake Solid?Liquid Separation Drying MELT CRYSTALLIZATION Characteristics of Melt Crystallization Processes of Melt Crystallization Postcrystallization Treatments Laboratory Techniques EXAMPLES OF REALIZED CONTINUOUS CRYSTALLIZATION PROCESSES Choosing the Drain Point in Process Design Example Crop Crystallization for Organic Compounds Example Crystallization of Table Salt Results DESIGN EXAMPLES OF MELT CRYSTALLIZATION Concepts of Melt Crystallization Outlook INDEX
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