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Preface |
6 |
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Contents |
8 |
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Part I: Process-Spray Micro Scale: Elementary Processes at Phase Boundaries |
11 |
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Chapter 1: Investigation of Elementary Processes of Non-Newtonian Droplets Inside Spray Processes by Means of Direct Numerical... |
12 |
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1.1 Introduction |
15 |
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1.2 Mathematical Modeling |
16 |
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1.2.1 Governing Equations |
16 |
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1.2.2 Basics of VOF Method |
18 |
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1.3 Results and Discussion |
19 |
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1.3.1 Lamella Stabilization |
19 |
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1.3.1.1 Head-On Collisions |
20 |
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1.3.1.2 Off-Center Collisions |
22 |
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1.3.2 Collision of Shear-Thinning Droplets |
25 |
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1.3.2.1 Head-On Collisions |
26 |
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1.3.2.2 Off-Center Collisions |
30 |
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1.3.3 Collision of Non-isoviscous Droplets |
34 |
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1.3.3.1 Modeling of Non-isoviscous Flow |
35 |
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1.3.3.2 Coalescence Suppression Algorithm |
36 |
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1.3.3.3 Collision of Equal Sized Droplets |
37 |
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1.3.3.4 Collision of Unequal Sized Droplets |
39 |
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1.3.4 Collision of Viscoelastic Droplets |
43 |
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1.3.4.1 Numerical Methods for Viscoelastic Flows |
45 |
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1.3.4.2 Simulation of Head-On and Off-Center Collisions |
46 |
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1.3.5 Mechanistic Modeling of the Collision of Viscous Droplets |
49 |
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1.3.5.1 Model Extension |
51 |
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1.3.5.2 Validation |
52 |
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1.3.5.3 Hybrid Model |
54 |
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1.4 Summary and Outlook |
57 |
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References |
58 |
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Chapter 2: Interfacial Engineering for the Microencapsulation of Lipophilic Ingredients by Spray-Drying |
61 |
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2.1 Introduction |
62 |
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2.2 Materials and Methods |
65 |
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2.3 Results and Discussion |
69 |
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2.4 Process Windows for beta-Lactoglobulin-Stabilised Emulsions |
69 |
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2.5 Impact of Protein Hydrolysis on the Interfacial Properties of beta-Lactoglobulin |
73 |
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2.6 When Limiting the Degree of Hydrolysis Good Encapsulation Properties May Be Achieved. Peptides at the Interface Reduce Aut... |
79 |
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2.7 Controlled Fibril Formation for the Stabilisation of the Oil-Water Interface and Enhancement of the Functionality of Spray... |
82 |
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2.8 Bilayer Emulsions with Pectin as Poly-Anion Are Stable During Atomisation and Drying |
84 |
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2.8.1 Molecular Structure of Pectin |
84 |
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2.9 Conclusion |
89 |
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References |
90 |
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Chapter 3: Structure Formation within Spray-Dried Droplets |
96 |
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3.1 Introduction |
98 |
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3.2 Modelling of Morphology Evolution Using Mesh-free Methods |
100 |
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3.3 The Smoothed Particle Hydrodynamics Method |
101 |
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3.4 Modelling Droplet Drying Using SPH |
103 |
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3.5 Modelling Morphology Evolution Within a Single Slurry Droplet by SPH |
104 |
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3.6 Representation of Primary Particles Within a Slurry |
106 |
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3.7 Surface Tension and Contact Angle |
107 |
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3.8 Simulation with a Constant Drying Rate (First Drying Period) |
108 |
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3.9 Model Extension to the Second Drying Period |
112 |
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3.10 Diffusion-Driven Drying of a Porous Structure and Coupling of SPH with a Grid-Based Method |
117 |
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3.11 A Mathematical Model of Spray Polymerisation and Reactive Spray Drying |
119 |
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3.12 Numerical Simulations of Spray Polymerisation |
122 |
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3.13 Conclusion and Outlook |
129 |
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References |
130 |
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Chapter 4: Acoustic Levitation: A Powerful Tool to Model Spray Processes |
133 |
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4.1 Introduction |
135 |
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4.2 Principles of the Acoustic Levitation |
137 |
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4.3 Material and Methods |
138 |
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4.3.1 Levitator Setup |
138 |
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4.3.2 Visualization Methods |
140 |
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4.3.3 Droplet Generation |
140 |
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4.3.4 Particle Removal |
141 |
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4.3.5 Raman Spectroscopy |
142 |
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4.3.6 Automatization |
142 |
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4.3.7 Substance Systems |
143 |
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4.4 Results and Discussion |
144 |
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4.4.1 Validation of the Simulated Fluid Dynamics Inside the Levitator |
144 |
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4.5 Reactive Systems |
148 |
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4.5.1 Polymerization of N-Vinyl-2-Pyrrolidone to Polyvinylpyrrolidone |
148 |
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4.5.1.1 Conversion Tracking by Raman Spectroscopy |
148 |
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4.5.1.2 Particle Morphology |
153 |
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4.5.2 Polymerization of Sodium Acrylate |
155 |
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4.5.3 Polymerization of Partially Neutralized Acrylic Acid |
157 |
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4.5.3.1 Process Properties |
157 |
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4.5.3.2 Particle Properties |
161 |
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4.6 Nonreactive System |
164 |
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4.6.1 Mannitol |
164 |
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4.6.1.1 Evaporation Process |
164 |
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4.6.1.2 Particle Morphology |
167 |
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4.7 Conclusions |
171 |
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4.8 Outlook |
172 |
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References |
172 |
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Chapter 5: Movement and Hydrodynamic Instabilities of Particle-Laden Liquid Jets in the Centrifugal Field Influenced by a Gas ... |
176 |
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5.1 Introduction |
179 |
|
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5.2 Physical-Mathematical Modeling |
181 |
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5.3 Time Steady Flow |
183 |
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5.4 Perturbation Analysis |
189 |
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5.5 Experiments |
195 |
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5.6 Experimental Results |
198 |
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5.7 Calculation Results and Comparison |
201 |
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5.8 Conclusion |
206 |
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5.9 Acknowledgment |
207 |
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References |
207 |
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|
Chapter 6: Experimental Investigation and Modeling of Coalescence and Agglomeration for Spray Drying of Solutions |
210 |
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6.1 Introduction |
211 |
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6.2 Material and Methods (Low Viscosity) |
214 |
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6.2.1 Experimental Setup |
214 |
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6.2.2 Liquid Properties |
216 |
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|
6.3 Results and Discussion (Low Viscosity) |
217 |
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6.3.1 Collision Maps of Low-Viscous Liquids |
217 |
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|
6.3.2 Satellite Droplet Formation with K30 Solutions |
223 |
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|
6.4 Material and Methods (High Viscosity) |
226 |
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|
6.4.1 Drop Generator for High-Viscous Liquids |
226 |
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|
6.4.2 Liquid Properties |
227 |
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|
6.5 Results and Discussion (High Viscosity) |
228 |
|
|
6.5.1 Performance of the HiDrip Drop Generator |
228 |
|
|
6.5.2 Collision Maps of High-Viscous Liquids |
230 |
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6.6 Methods and Materials (Different Viscosities) |
232 |
|
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6.7 Results and Discussion (Different Viscosities) |
233 |
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6.8 Conclusions |
235 |
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References |
237 |
|
|
Chapter 7: Particle Formation from Gas-Enriched Polymeric Melts and Polymeric Solutions |
239 |
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7.1 Introduction |
240 |
|
|
7.2 Material and Methods |
241 |
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|
7.2.1 Material |
241 |
|
|
7.2.1.1 Carbon Dioxide |
241 |
|
|
7.2.1.2 Water |
241 |
|
|
7.2.1.3 Polyethyleneglycol (PEG 6000) |
241 |
|
|
7.2.1.4 Polyvinylpyrrolidone (K30 and K90) |
242 |
|
|
7.2.2 Methods |
242 |
|
|
7.2.2.1 Spray Experiments |
242 |
|
|
7.2.2.2 Lab Scale Plant |
242 |
|
|
7.2.2.3 Pilot Scale Plant |
243 |
|
|
7.2.2.4 Experiments in a High-Pressure View Cell |
245 |
|
|
7.2.2.5 Thermography |
246 |
|
|
7.3 Results and Discussion |
246 |
|
|
7.3.1 Experiments Using a High-Pressure View Cell |
246 |
|
|
7.3.1.1 Phase Behavior of Aqueous PVP K30 Solution and CO2 |
246 |
|
|
7.3.1.2 Phase Equilibrium |
247 |
|
|
7.3.2 Spray Experiments (Saturated and Undersaturated Solutions) |
247 |
|
|
7.3.2.1 Experiments with Flat Jet Nozzles |
248 |
|
|
7.3.2.2 Experiments with Orifices and Capillaries |
251 |
|
|
7.3.2.3 Experiments Using an Optically Transparent Capillary (Flow Observations) |
255 |
|
|
7.3.3 Estimation of the Flow Regime of the Resulting Two Phase Flow in a Capillary |
258 |
|
|
7.3.3.1 Deductions for the Continuously Working Process |
260 |
|
|
7.3.4 Spray Experiments (with an Excess of CO2) |
261 |
|
|
7.3.4.1 Experiments Using an Optically Transparent Capillary (Flow Observations) |
261 |
|
|
7.3.4.2 Powder Generation of PEG 6000 |
262 |
|
|
7.3.4.3 Powder Generation of PVP (K30 and K90) |
264 |
|
|
7.3.4.4 Thermography |
264 |
|
|
7.4 Summary |
267 |
|
|
References |
268 |
|
|
Chapter 8: A Real-Time Process Analysis System for the Simultaneous Acquisition of Spray Characteristics |
269 |
|
|
8.1 Introduction |
269 |
|
|
8.2 Real-Time Process Analysis System |
272 |
|
|
8.2.1 Goals |
272 |
|
|
8.2.2 Architecture of the Real-Time Process Analysis System on the System Level |
275 |
|
|
8.2.2.1 Choosing a Computing Platform for the Image-Processing Hardware |
276 |
|
|
Evaluation Summary |
279 |
|
|
8.3 Image-Processing Methods for Droplet and Particle Measurement |
280 |
|
|
8.3.1 A Novel Connected Components Analysis Algorithm |
281 |
|
|
8.3.1.1 Data Structures, Operations, and Parameters |
281 |
|
|
8.3.1.2 Algorithmic Description |
283 |
|
|
8.3.2 A Novel Connected Components Analysis Architecture |
286 |
|
|
8.3.2.1 Global Merger Patterns |
287 |
|
|
8.3.2.2 Coalescing Unit |
289 |
|
|
8.3.2.3 Evaluation of the CCA Architecture |
290 |
|
|
8.4 Filament Formation |
291 |
|
|
8.5 Droplet Collisions |
294 |
|
|
8.6 Shape of Non-spherical Particles |
296 |
|
|
8.7 Analysis of Droplet Jets |
298 |
|
|
8.8 Measuring the Interfacial Tension of a Pendant Droplet |
300 |
|
|
8.9 Characterization of Dynamic Spray Processes |
303 |
|
|
8.10 Conclusion |
305 |
|
|
References |
305 |
|
|
Part II: Process-Spray Meso Scale: Process Analysis, Modeling and Scaling |
310 |
|
|
Chapter 9: Modeling and Simulation of Single Particle and Spray Drying of PVP- and Mannitol-Water in Hot Air |
311 |
|
|
9.1 Introduction |
312 |
|
|
9.2 Single Bi-component Droplet Drying |
313 |
|
|
9.2.1 Mathematical Model |
314 |
|
|
9.2.2 Results and Discussion |
319 |
|
|
9.2.2.1 Particle Expansion |
322 |
|
|
9.2.2.2 Design of Experiments |
325 |
|
|
9.2.3 Conclusions |
327 |
|
|
9.3 Spray Drying |
327 |
|
|
9.3.1 Mathematical Model |
328 |
|
|
9.3.2 Results and Discussion |
332 |
|
|
9.3.3 Conclusions |
338 |
|
|
9.4 Perspectives |
338 |
|
|
References |
339 |
|
|
Chapter 10: Droplet-Stream Freeze-Drying for the Production of Protein Formulations: From Simulation to Production |
342 |
|
|
10.1 Introduction |
345 |
|
|
10.2 Methods |
346 |
|
|
10.2.1 Spray Solutions |
346 |
|
|
10.2.2 Spray-Drying |
346 |
|
|
10.2.3 Spray-Freeze-Drying |
346 |
|
|
10.2.3.1 Droplet Generation |
346 |
|
|
10.2.3.2 Stroboscopic and High-Speed Camera Recordings |
347 |
|
|
10.2.3.3 Droplet Freezing |
348 |
|
|
10.2.3.4 Droplet Drying |
349 |
|
|
10.2.3.5 Acoustic Levitator |
350 |
|
|
10.2.4 Particle Analysis |
351 |
|
|
10.2.5 Numerical Simulations |
351 |
|
|
10.2.5.1 Hybrid Simulations of Fluid Flow and Temperature Field |
352 |
|
|
10.2.5.2 Thermal Lattice-Boltzmann Method |
353 |
|
|
10.2.5.3 Lagrangian Model for Drying of Frozen Particles |
356 |
|
|
10.3 Results and Achievements |
359 |
|
|
10.3.1 Droplet Generation |
359 |
|
|
10.3.2 Collisions and Coalescence in Fast Streams of Small Droplets |
359 |
|
|
10.3.3 Droplet Freezing |
362 |
|
|
10.3.3.1 Droplet Freezing in Stagnant Cold Air |
362 |
|
|
10.3.3.2 Droplet Freezing in a Cold, N2 -GasVortex |
362 |
|
|
10.3.3.3 Jet-Vortex-Freezer |
364 |
|
|
10.3.4 Drying |
364 |
|
|
10.3.5 Dosage Forms |
365 |
|
|
10.3.6 Numerical Simulations |
368 |
|
|
10.3.6.1 Isothermal Flow About Porous Particles |
368 |
|
|
10.3.6.2 Test Cases for Thermal LBM |
375 |
|
|
10.3.6.3 Validation of the Drying Model |
379 |
|
|
References |
380 |
|
|
Chapter 11: Correlations Between Suspension Formulation, Drying Parameters, Granule Structure, and Mechanical Properties of Sp... |
383 |
|
|
11.1 Introduction |
384 |
|
|
11.2 Material and Methods |
386 |
|
|
11.3 Method Development for Internal Structure Preparation and Quantification |
389 |
|
|
11.3.1 Model Granules for Characterization Tasks |
389 |
|
|
11.3.2 Internal Structure Preparation and Visualization |
390 |
|
|
11.3.3 Internal Structure Quantification on Micro- and Macrostructure Level |
392 |
|
|
11.3.4 Evaluation of Binder Distribution |
395 |
|
|
11.3.5 Alternative Structure Visualization Techniques: Opportunities and Threads |
398 |
|
|
11.4 Variation of Internal Granule Structure Via Suspension Formulation and Process Parameters |
400 |
|
|
11.4.1 Investigated Parameters: Experimental Design |
400 |
|
|
11.4.2 Effect of Changed Suspension Formulation on Suspension Properties and Resulting Internal Granule Structures |
402 |
|
|
11.4.2.1 Variation of Solid Content |
402 |
|
|
11.4.2.2 Variation of Primary Particle Size |
403 |
|
|
11.4.2.3 Variation of Suspension Temperature |
408 |
|
|
11.4.2.4 Variation of Suspension pH Value |
409 |
|
|
11.4.2.5 Variation of Additive Type |
413 |
|
|
11.4.2.6 Variation of Additive Amount |
419 |
|
|
11.4.2.7 Summary: Effect of Varied Suspension Formulation on Suspension Properties and Resulting Internal Granule Structures |
420 |
|
|
11.4.3 Effect of Changed Process Parameters on Resulting Internal Granule Structures |
423 |
|
|
11.4.3.1 Pretests Regarding Droplet Size Determination Using External Nozzle Test Stand |
424 |
|
|
11.4.3.2 Effect of Nozzle Gas Mass Flow, Suspension Mass Flow, and Drying Temperature: Analysis Using Design of Experiments DoE |
427 |
|
|
Suspension 1:3wt% Additive Component |
428 |
|
|
Suspension 2: No Additive Component |
431 |
|
|
11.4.3.3 Further Examples for Varied Process Parameters |
433 |
|
|
Variation of Drying Kinetics |
436 |
|
|
Variation of Atomizer Type |
438 |
|
|
11.4.3.4 Summary |
442 |
|
|
11.4.4 Single Droplet Drying Experiments Regarding Influencing Internal Structure Development Via Suspension Formulation and P... |
442 |
|
|
11.5 Conclusion: Correlations Between Internal Structure Parameters and Mechanical Properties |
444 |
|
|
References |
447 |
|
|
Chapter 12: Statistical Extinction Method for the Inline Monitoring of Particle Processes |
449 |
|
|
12.1 Introduction |
450 |
|
|
12.2 Statistical Extinction Method |
452 |
|
|
12.3 Advanced Statistical Extinction Method |
455 |
|
|
12.4 Simulation Model for the Extinction of Light Beams |
457 |
|
|
12.5 Particle Arrangement in a Light Beam |
459 |
|
|
12.6 Influence of the Distribution of the Light Intensity |
461 |
|
|
12.7 Influence of the Aperture of the Detector Optic |
463 |
|
|
12.8 Influence of the Polydispersity of a Particle Collective |
464 |
|
|
12.9 Optical Principles of the SE-Sensor |
467 |
|
|
12.10 Optical Principle of the PSD-SE-Sensor |
471 |
|
|
12.11 One-Piece vs. Two-Piece Sensor Concept for Process Plants |
472 |
|
|
12.12 Sensor Designs of the SE-Sensor for the Investigation of Different Particle Processes |
475 |
|
|
12.13 Sensor Design of the PSD-SE-Sensor for the Investigation of Particle Processes |
475 |
|
|
12.14 Measurement Range and Measurement Uncertainty of the SE-Method |
477 |
|
|
12.15 Validation of the SE-Method with Monodisperse Particles |
479 |
|
|
12.16 Investigation of Polydisperse Spray Processes with the SE-Method |
482 |
|
|
12.17 Investigation of Spray Processes with the PSD-SE-Sensor |
485 |
|
|
12.18 Summary and Conclusions |
488 |
|
|
References |
490 |
|
|
Chapter 13: Numerical Simulation of Monodispersed Droplet Generation in Nozzles |
492 |
|
|
13.1 Introduction |
493 |
|
|
13.2 Mathematical Model |
495 |
|
|
13.2.1 Level Set Method |
496 |
|
|
13.2.2 Treatment of Surface Tension Effects |
498 |
|
|
13.2.3 New Generation Mesh Deformation Technique |
499 |
|
|
13.2.4 Discrete Projection Method (DPM) |
501 |
|
|
13.3 Numerical Results |
504 |
|
|
13.3.1 Rising Bubble |
504 |
|
|
13.3.2 Simulation of Laminar Jet Breakup: Dripping |
505 |
|
|
13.3.3 Simulation of Laminar Jet Breakup: Jetting |
508 |
|
|
13.3.4 Simulation of Laminar Jets: Coiling |
509 |
|
|
13.3.5 Oscillating Non-Newtonian Droplet Simulations |
510 |
|
|
13.3.6 Simulation of Encapsulation Processes |
512 |
|
|
References |
514 |
|
|
Chapter 14: Spray Drying Tailored Mannitol Carrier Particles for Dry Powder Inhalation with Differently Shaped Active Pharmace... |
516 |
|
|
14.1 Introduction |
517 |
|
|
14.2 Material and Methods |
519 |
|
|
14.2.1 Materials |
519 |
|
|
14.2.2 Spray Drying of Mannitol |
520 |
|
|
14.2.2.1 Droplet Size Experiments |
520 |
|
|
14.2.2.2 Pilot Scale Spray Dryer |
521 |
|
|
Early Experimental Setup |
521 |
|
|
Improved Experimental Setup |
521 |
|
|
14.2.2.3 Hot Stage Microscopy |
522 |
|
|
14.2.2.4 Droplet Size Analysis |
522 |
|
|
14.2.2.5 Design of Experiments |
522 |
|
|
14.2.2.6 Particle Size |
523 |
|
|
14.2.2.7 Particle Visualisation |
523 |
|
|
14.2.2.8 Particle Morphology |
524 |
|
|
Survey for Particle Shape and Surface Roughness |
524 |
|
|
Particle Cross Sections |
524 |
|
|
Surface Roughness by SEM Evaluation |
525 |
|
|
Particle Shape by Image Analysis |
525 |
|
|
14.2.2.9 Flowability |
525 |
|
|
14.2.2.10 Brunauer-Emmett-Teller (BET) Surface Area |
526 |
|
|
14.2.2.11 Breaking Strength |
526 |
|
|
14.2.2.12 Mercury Intrusion Porosity (MIP) |
526 |
|
|
14.2.2.13 X-Ray Powder Diffraction |
527 |
|
|
14.2.3 Simulation of the Drying of Bi-component Droplets |
527 |
|
|
14.2.4 Drug Preparation |
527 |
|
|
14.2.4.1 Jet Mill Micronisation of Model Drugs |
528 |
|
|
14.2.4.2 Spray Drying of Model Drugs |
528 |
|
|
14.2.4.3 Particle Size |
528 |
|
|
14.2.4.4 X-Ray Powder Diffraction |
528 |
|
|
14.2.4.5 Visualisation |
529 |
|
|
14.2.5 Preparation of Interactive Powder Blends |
529 |
|
|
14.2.5.1 Blending of Mannitol and Drug |
529 |
|
|
14.2.5.2 Drug Localisation by Confocal Raman Analysis |
529 |
|
|
14.2.5.3 Blend Homogeneity |
530 |
|
|
14.2.5.4 Drug Quantification |
530 |
|
|
14.2.6 Aerodynamic Characterisation |
531 |
|
|
14.2.6.1 Assessment of Fine Particles |
531 |
|
|
14.2.6.2 Drug Quantification |
532 |
|
|
14.3 Results and Discussion |
532 |
|
|
14.3.1 Impact of Droplet Size on the Drying of Mannitol |
532 |
|
|
14.3.2 Hot Stage Microscopy to Elucidate the Drying of Mannitol |
533 |
|
|
14.3.3 Spray Drying of Mannitol: Pilot Scale |
535 |
|
|
14.3.3.1 Design of Experiments: Power of the Model |
536 |
|
|
14.3.3.2 Particle Size |
536 |
|
|
14.3.3.3 Particle Morphology |
539 |
|
|
Particle Shape |
539 |
|
|
Surface Roughness |
542 |
|
|
14.3.3.4 Flowability |
544 |
|
|
14.3.3.5 BET Surface Area |
545 |
|
|
14.3.3.6 Breaking Strength |
545 |
|
|
14.3.3.7 Mercury Intrusion Porosimetry (MIP) |
546 |
|
|
14.3.3.8 Crystallinity |
547 |
|
|
14.3.4 Simulation of the Drying of Bi-component Droplets |
547 |
|
|
14.3.5 Drug Quality and Carrier Selection |
548 |
|
|
14.3.6 Aerodynamic Characterisation |
551 |
|
|
14.3.6.1 Micronised SBS Quality |
552 |
|
|
14.3.6.2 Spray Dried SBS Quality |
553 |
|
|
Correlation of Particle Shape and FPF |
553 |
|
|
Correlation of Surface Roughness and FPF |
556 |
|
|
Correlation of Particle Size and FPF |
558 |
|
|
Correlation of Flowability and FPF |
559 |
|
|
14.3.6.3 Correlation of Spray Drying Parameters and DPI Performance |
560 |
|
|
14.3.6.4 Transferability to Other Drugs: Blends with Budesonide |
560 |
|
|
14.4 Conclusions |
561 |
|
|
References |
562 |
|
|
Chapter 15: Pulverisation of Emulsions with Supercritical CO2 |
566 |
|
|
15.1 Introduction |
567 |
|
|
15.2 Materials |
567 |
|
|
15.3 Thermodynamic Properties of the Investigated Liquids |
568 |
|
|
15.3.1 Experimental Procedures |
568 |
|
|
15.3.1.1 Solubility Measurements |
568 |
|
|
15.3.1.2 Viscosity and Density Measurements |
569 |
|
|
15.3.1.3 Interfacial Tension Measurements |
571 |
|
|
15.3.2 Results |
573 |
|
|
15.3.2.1 Solubility |
573 |
|
|
15.3.2.2 Viscosity |
578 |
|
|
15.3.2.3 Density |
581 |
|
|
15.3.2.4 Interfacial Tension |
584 |
|
|
15.3.3 Spray Behaviour and Powder Production |
588 |
|
|
15.3.3.1 Experimental Procedure |
588 |
|
|
15.3.4 Results |
591 |
|
|
15.3.4.1 Disintegration of Pure and Gas-Saturated Liquid Sheets |
591 |
|
|
15.3.4.2 Powder Characteristics |
598 |
|
|
15.4 Conclusions |
603 |
|
|
References |
605 |
|
|
Chapter 16: Superheated Atomization |
608 |
|
|
16.1 Introduction |
610 |
|
|
16.2 Material and Methods |
611 |
|
|
16.2.1 Test Facility and Nozzles |
611 |
|
|
16.2.2 Measurement Devices |
614 |
|
|
16.2.3 Sprayed Fluids |
615 |
|
|
16.3 Results |
619 |
|
|
16.3.1 Characteristics Inside the Nozzle |
619 |
|
|
16.3.2 Spray Characteristics |
625 |
|
|
16.4 Discussion |
635 |
|
|
16.5 Conclusion |
642 |
|
|
References |
643 |
|
|
Chapter 17: Direct Numerical Simulations of Shear-Thinning Liquid Jets and Droplets |
645 |
|
|
17.1 Introduction |
646 |
|
|
17.2 Numerical Method |
648 |
|
|
17.3 Viscosity Model and Material Properties |
649 |
|
|
17.4 Investigation of a PVP Solution Liquid Jet |
651 |
|
|
17.5 Investigation of Praestol Jets |
656 |
|
|
17.6 Investigation of Droplet Oscillations |
664 |
|
|
17.7 Conclusion |
673 |
|
|
References |
675 |
|
|
Chapter 18: IntegralProcess Modelling and Simulation for Solid-Particle-Forming Spray Processes |
677 |
|
|
18.1 Introduction |
679 |
|
|
18.2 Jet/Sheet Fragmentation Model |
681 |
|
|
18.2.1 Volume of Fluid Method |
681 |
|
|
18.2.2 Numerical Simulation of Liquid Sheet Fragmentation Process |
682 |
|
|
18.2.2.1 Case Setup |
682 |
|
|
18.2.2.2 Liquid Sheet Disintegration |
686 |
|
|
18.2.2.3 Liquid Sheet Breakup Length |
687 |
|
|
18.2.2.4 Primary Droplet Size and Velocity |
688 |
|
|
18.3 Droplet Breakup Model |
690 |
|
|
18.3.1 Empirical Models |
692 |
|
|
18.3.2 Droplet-Deformation-Based Models |
693 |
|
|
18.3.2.1 TAB Model |
693 |
|
|
18.3.2.2 ETAB Model |
694 |
|
|
18.3.3 Validation: Melt Atomization Process |
695 |
|
|
18.3.3.1 Case Setup |
696 |
|
|
18.3.3.2 Gas Flow Dynamics |
700 |
|
|
18.3.3.3 Pressure-Swirl Atomization Process |
701 |
|
|
18.3.3.4 Free-Fall Atomization Process |
705 |
|
|
18.4 Heat Transfer and Solidification Model |
706 |
|
|
18.5 Particle-Droplet Collision Model |
709 |
|
|
18.5.1 Collision Number |
709 |
|
|
18.5.2 Collision Efficiency |
710 |
|
|
18.5.2.1 Case Setup |
711 |
|
|
18.5.2.2 Gas Flow Dynamics |
712 |
|
|
18.5.2.3 Collision Efficiency |
712 |
|
|
18.6 Particle Penetration Model |
715 |
|
|
18.6.1 Force Balance Approach |
716 |
|
|
18.6.2 CFD Model Description |
717 |
|
|
18.6.2.1 Volume of Fluid Method |
717 |
|
|
18.6.2.2 Six-DoF Method |
717 |
|
|
18.6.2.3 Dynamic Mesh Technique |
718 |
|
|
18.6.3 Penetration Model Validation |
719 |
|
|
18.6.4 CFD Penetration Model Results and Discussion |
723 |
|
|
18.6.4.1 Case Setup |
723 |
|
|
18.6.4.2 Collision Outcomes |
724 |
|
|
18.6.4.3 Re-We Regime Maps for Particle Penetration |
726 |
|
|
18.7 Multiscale Modelling Spray Processing of Composite Particles |
730 |
|
|
18.7.1 Particle-Droplet Mixing Behaviour (Macro-scale) |
732 |
|
|
18.7.2 Particle-Droplet Collision Behaviour (Mesoscale) |
733 |
|
|
18.7.3 Particle Penetration Behaviour (Micro-scale) |
737 |
|
|
18.7.3.1 Apparent Viscosity |
737 |
|
|
18.7.3.2 Critical Penetration Velocity |
738 |
|
|
18.7.3.3 Incorporation Efficiency and Sticking Efficiency |
741 |
|
|
18.8 Summary and Conclusions |
743 |
|
|
References |
743 |
|
|
Part III: Process-Spray Macro Scale: Process Function, Particle and Powder Properties |
747 |
|
|
Chapter 19: Hot Gas Atomization of Complex Liquids for Powder Production |
748 |
|
|
19.1 Introduction |
749 |
|
|
19.2 Material and Methods |
752 |
|
|
19.3 Hot Gas Atomization Setup: Hot Gas Nozzle Characteristics and Implementation of Hot Gas Nozzle into the Spray Tower |
754 |
|
|
19.4 Basic Flow and Temperature Field in the Spray Tower |
758 |
|
|
19.5 Atomization Characteristics and Spray Propagation |
765 |
|
|
19.6 Drying of PVP Solutions in Hot Gas Atomization Process |
768 |
|
|
19.7 Impact on Droplet Clustering on Heat Transfer Within the Spray |
770 |
|
|
19.7.1 Numerical Setup for Prediction of Spray Propagation with Large-Eddy Simulation |
770 |
|
|
19.8 Results: Particle Clustering |
773 |
|
|
19.9 Impact of Spray Chamber Design and Atomizer Gas Pressure on Cluster Sizes |
779 |
|
|
19.10 Correlation of the Droplet-Gas Interaction |
783 |
|
|
19.11 Summary and Conclusions |
787 |
|
|
References |
788 |
|
|
Chapter 20: Polymerization in Sprays: Atomization and Product Design of Reactive Polymer Solutions |
792 |
|
|
20.1 Introduction |
794 |
|
|
20.2 Material and Methods: Atomization of Polymer Solutions |
798 |
|
|
20.3 Results of the Atomization of Polymer Solutions |
803 |
|
|
20.4 Material and Methods: Rheokinetics |
813 |
|
|
20.5 Results of the Rheokinetics |
820 |
|
|
20.6 Pre-reaction Within the Nozzle |
827 |
|
|
20.7 Conclusion |
834 |
|
|
References |
835 |
|
|
Chapter 21: Investigation on the Usage of Effervescent Atomization for Spraying and Spray Drying of Rheological Complex Food L... |
839 |
|
|
21.1 Introduction |
841 |
|
|
21.2 Material and Methods |
841 |
|
|
21.2.1 Model Systems |
841 |
|
|
21.2.2 Polyvinylpyrrolidone |
841 |
|
|
21.2.3 Maltodextrin |
845 |
|
|
21.2.4 Emulsions |
847 |
|
|
21.2.5 Effervescent Atomizer |
852 |
|
|
21.2.6 Conventional Atomizers |
853 |
|
|
21.2.7 Two-Phase Flow Inside an Effervescent Atomizer |
854 |
|
|
21.2.8 Test Rig |
855 |
|
|
21.2.9 Modeling of Spray Drop Sizes |
857 |
|
|
21.2.10 Abel Inversion |
859 |
|
|
21.2.11 Spray Dryer |
860 |
|
|
21.3 Results, Achievements, and Discussion/Conclusions |
861 |
|
|
21.3.1 Flow Pattern Inside the Atomizer |
861 |
|
|
21.3.2 Flow Pattern Inside the Nozzle Orifice |
866 |
|
|
21.3.3 Spray Characteristics |
866 |
|
|
21.3.3.1 Spray Structure |
866 |
|
|
21.3.3.2 Spray Drop Sizes of Single-Phase Feeds |
870 |
|
|
21.3.3.3 Spray Drop Sizes of Multiphase Feeds |
880 |
|
|
21.3.3.4 Pulsation of Spray |
883 |
|
|
21.3.3.5 Predicted Spray Drop Size |
883 |
|
|
21.3.3.6 Local Spray Drop Sizes |
885 |
|
|
21.3.4 Oil Drop Size |
886 |
|
|
21.3.5 Spray Drying of PVP K30 Solutions |
891 |
|
|
21.4 Conclusion |
895 |
|
|
References |
895 |
|
|
Chapter 22: Experimental Evaluation and Control of Interaction of Gas Environment and Rotary Atomized Spray for Production of ... |
899 |
|
|
22.1 Introduction |
901 |
|
|
22.1.1 Spraying of Liquid |
902 |
|
|
22.1.2 Laminar Operating Rotary Atomizer |
902 |
|
|
22.1.3 Similarity Trials |
904 |
|
|
22.1.4 Objective |
906 |
|
|
22.2 Breakup of Stretched Liquid Threads Influenced by Cross-Wind Flow: Similarity Trials |
906 |
|
|
22.2.1 Theory |
906 |
|
|
22.2.2 Material and Method |
908 |
|
|
22.2.3 Experimental Results: Breakup Length |
909 |
|
|
22.2.4 Experimental Results: Mean Drop Size |
912 |
|
|
22.2.5 Experimental Results: Drop Size Distribution |
916 |
|
|
22.3 Design of Gas-Distribution System |
918 |
|
|
22.3.1 Flow Simulation Theory |
919 |
|
|
22.3.2 Gas-Distribution Concept |
919 |
|
|
22.3.3 Realization of the Gas Distributor´s Concept |
920 |
|
|
22.4 Optimization of the LamRot Spraying Device |
924 |
|
|
22.4.1 Direction of Thread Propagation |
925 |
|
|
22.4.2 Avoiding Sedimentation |
927 |
|
|
22.4.3 Assistance of Swirl Flow by the LamRot Design |
927 |
|
|
22.5 Proving of the Gas-Distribution Concept |
928 |
|
|
22.5.1 Spray Drying of PVP Solution |
929 |
|
|
22.5.2 Spray Drying of Mannitol |
931 |
|
|
22.6 Conclusion |
933 |
|
|
References |
934 |
|
|
Chapter 23: Processing of Functional Capsule Powder Particles Based on Multiple Emulsions Using a Prilling Process |
937 |
|
|
23.1 Introduction |
939 |
|
|
23.2 Materials and Methods |
943 |
|
|
23.2.1 Materials |
943 |
|
|
23.2.1.1 Watery Phases |
943 |
|
|
23.2.1.2 Oil Phases |
943 |
|
|
23.2.1.3 Surfactants |
943 |
|
|
23.2.1.4 Thickener |
944 |
|
|
23.2.1.5 Model Emulsion Systems and Their Compositions |
944 |
|
|
23.2.1.6 Materials for Iron Release Experiment |
944 |
|
|
23.2.2 Analytical Methods and Procedures and Selected Analytical Results |
944 |
|
|
23.2.2.1 Shear Viscosity of Emulsions |
946 |
|
|
23.2.2.2 Viscoelasticity of Emulsions |
948 |
|
|
23.2.2.3 Extensional Viscosity of Emulsions |
949 |
|
|
23.2.2.4 Surface Tension sigma |
950 |
|
|
23.2.2.5 Interfacial Tension gamma (O/W and W/O/W Emulsions) |
951 |
|
|
23.2.3 Processing Procedures and Conditions |
953 |
|
|
23.2.3.1 Emulsion Preparation |
953 |
|
|
SE Preparation Using Rotor-Stator System |
953 |
|
|
DE Preparation Using Rotating Membrane |
953 |
|
|
23.2.3.2 Spray Processing Experiments Using Air-Assisted Atomizer |
954 |
|
|
Experimental Setup |
954 |
|
|
Spray Processing of DE with Functional Tracer |
955 |
|
|
Emulsion Prilling Experiments |
956 |
|
|
23.2.3.3 Spraying of Emulsions Applying a Novel ROtary Pressure ATomizer (ROPAT) |
956 |
|
|
23.2.3.4 Iron Release Experiment Setup and Procedure |
957 |
|
|
23.3 Results, Achievements, and Discussion/Conclusions |
958 |
|
|
23.3.1 Spray Processing: Structural Preservation Criterion (Process-Structure Relation) |
958 |
|
|
23.3.1.1 Influence of Spray Process Parameters on Secondary Droplets (3AT Nozzles) |
959 |
|
|
Impact of Gas/Liquid Ratio on SE Structure |
960 |
|
|
Impact of GLR on DE Structure |
961 |
|
|
Impact of Pure Liquid-Cap Nozzle Flow on Secondary Droplet Size of SE, DE |
963 |
|
|
Two-Phase Flow Impact on Secondary Droplet Size of SE, DE in 3AT Nozzles |
968 |
|
|
Impact of Spray Processing on Tertiary Emulsion Droplet/Spray Particle Size |
971 |
|
|
Spraying of DE (W1/O/W2) and Release of Tracer into Continuous Phase |
974 |
|
|
23.3.1.2 Rotary Pressure Atomization a Mechanically Gentle Alternative (ROPAT Nozzle) |
976 |
|
|
23.4 Conclusions/Summary |
977 |
|
|
Bibliography |
979 |
|
|
Chapter 24: Analysis of Mechanisms for PVP-Active-Agent Formulation as in Supercritical Antisolvent Spray Process |
982 |
|
|
24.1 Introduction |
983 |
|
|
24.2 Materials and Methods |
984 |
|
|
24.2.1 Material |
984 |
|
|
24.2.2 Antisolvent |
985 |
|
|
24.2.3 Solvents |
985 |
|
|
24.2.4 Solutes |
986 |
|
|
24.2.5 SAS Plant |
987 |
|
|
24.2.6 Saturation Measurements |
989 |
|
|
24.2.7 Elastic Light Scattering Setup |
990 |
|
|
24.2.8 Combined Elastic and Inelastic Scattering Light Setup |
993 |
|
|
24.2.9 Particle Analysis |
995 |
|
|
24.2.10 Dissolution Measurements |
997 |
|
|
24.3 Results and Discussion |
998 |
|
|
24.3.1 Solute Solubility Measurements of Certain Solutes |
999 |
|
|
24.3.2 Mixing Behavior of Certain Solvents |
1001 |
|
|
24.3.3 Generation of Amorphous PVP Particles |
1006 |
|
|
24.3.4 Influence of Pressure and Concentration |
1007 |
|
|
24.3.5 Influence of the Solvent Composition |
1008 |
|
|
24.4 Generation of Paracetamol Crystals from EtOH, AC, and EtOH/AC Mixture Solutions |
1011 |
|
|
24.4.1 Ethanol Solutions |
1011 |
|
|
24.4.2 Acetone Solutions |
1013 |
|
|
24.4.3 Mixtures of Ethanol and Acetone |
1016 |
|
|
24.4.4 Generation of Solid Dispersions |
1019 |
|
|
24.4.5 PCM: PVP |
1019 |
|
|
24.4.6 PVP and Paracetamol (EtOH/AC=70/30 as Solvent) |
1020 |
|
|
24.4.7 Combined Elastic and Inelastic Scattered Light Measurements |
1023 |
|
|
24.5 Conclusion |
1025 |
|
|
References |
1027 |
|