Kinetics of Crystallization in Supersaturation

Kinetics of Crystallization in Supersaturation

Supersaturation Control Optimizes Crystal Size and Shape

Guide to Crystallization Development
Supersaturation Profiling
Non-Linear Cooling Rates for Constant Supersaturation
Automated Supersaturation Control
Particle Size Analysis for Process Optimization

Aplikace

Applications For Understanding Crystallization Kinetics

Optimization of Crystal Properties and Process Performance

Scientist recrystallize high value chemical compounds to obtain a crystal product with desired physical properties at optimal process efficiency. Seven steps are required to design the ideal recrystallization process from choosing the right solvent to obtaining a dry crystal product. This recrystallization guide explains step-by-step the procedure of developing a recrystallization process. It explains what information is required at each stage of recrystallization and outlines how to control critical process parameter

Solubility and Metastable Zone Width (mzw) Determination
The Building Blocks of Crystallization

Solubility curves are commonly used to illustrate the relationship between solubility, temperature, and solvent type. By plotting temperature vs. solubility, scientists can create the framework needed to develop the desired crystallization process. Once an appropriate solvent is chosen, the solubility curve becomes a critical tool for the development of an effective crystallization process.

Tvorba jader a růst krystalů
Hnací síla nukleace a růstu krystalů

Vědci a inženýři mají úplnou kontrolu nad celým procesem krystalizace díky možnosti přesného stanovení úrovně přesycení v průběhu procesu. Přesycení je hnací silou při tvorbě jader a růstu během krystalizace a rozhoduje o výsledné distribuci velikosti krystalů.

Measure Crystal Size Distribution
Improve Crystallization with Inline Particle Size, Shape, and Count Measurement

In-process probe-based technologies are applied to track particle size and shape changes at full concentration with no dilution or extraction necessary. By tracking the rate and degree of change to particles and crystals in real time, the correct process parameters for crystallization performance can be optimized.

Crystallization Seeding Protocol
Design and Optimize Seeding Protocol for Improved Batch Consistency

Seeding is one of the most critical steps in optimizing crystallization behavior. When designing a seeding strategy, parameters such as: seed size, seed loading (mass), and seed addition temperature must be considered. These parameters are generally optimized based on process kinetics and the desired final particle properties, and must remain consistent during scale-up and technology transfer.

Particle Engineering and Wet Milling
Control Particle Size With High Shear Wet Milling

Milling of dry powders can cause significant yield losses and can generate dust, creating health and safety hazards. In response to this, wet milling produces particles with a specifically designed size distribution. It is now common to employ high shear wet milling to break large primary crystals and agglomerates into fine particles.

Anti-Solvent Addition on Supersaturation
How Solvent Addition Can Control Crystal Size and Count

In an antisolvent crystallization, the solvent addition rate, addition location and mixing impact local supersaturation in a vessel or pipeline. Scientists and engineers modify crystal size and count by adjusting antisolvent addition protocol and the level of supersaturation.

Temperature Effects Crystallization Size and Shape
Supersaturation Control Optimizes Crystal Size and Shape

Crystallization kinetics are characterized in terms of two dominant processes, nucleation kinetics and growth kinetics, occurring during crystallization from solution. Nucleation kinetics describe the rate of formation of a stable nuclei. Growth kinetics define the rate at which a stable nuclei grows to a macroscopic crystal. Advanced techniques offer temperature control to modify supersaturation and crystal size and shape.

Temperature Effects Crystallization Size and Shape
Scaling-Up Agitation, Dosing, and Crystallization

Changing the scale or mixing conditions in a crystallizer can directly impact the kinetics of the crystallization process and the final crystal size. Heat and mass transfer effects are important to consider for cooling and antisolvent systems respectively, where temperature or concentration gradients can produce inhomogeneity in the prevailing level of supersaturation.

Chemical Process Development & Scale-Up
Design Robust and Sustainable Chemical Processes For Faster Transfer To Pilot Plant and Production

Design Robust and Sustainable Chemical Processes For Faster Transfer To Pilot Plant and Production

Chemical Reaction Kinetics Studies
Study Chemical Reaction Rates and Measure Kinetics Inline

In situ chemical reaction kinetics studies provide an improved understanding of reaction mechanism and pathway by providing concentration dependences of reacting components in real-time. Continuous data over the course of a reaction allows for the calculation of rate laws with fewer experiments due to the comprehensive nature of the data.  Reaction Progression Kinetics Analysis (RPKA) uses in situ data under synthetically relevant concentrations and captures information throughout the whole experiment ensuring that the complete reaction behavior can be accurately described.

Polymorphism Identification and Control
Understand Polymorphism and the Impact of Process Parameters

Polymorphism is a common phenomenon with many crystalline solids in the pharmaceutical and fine chemical industry. Scientists deliberately crystallize a desired polymorph to improve isolation properties, help overcome downstream process challenges, increase bioavailability or to prevent patent conflicts. Identifying polymorphic and morphological transformations in-situ and in real time eliminates unexpected process upset, out of specification product and costly reprocessing of material.

Scientist recrystallize high value chemical compounds to obtain a crystal product with desired physical properties at optimal process efficiency. Seven steps are required to design the ideal recrystallization process from choosing the right solvent to obtaining a dry crystal product. This recrystallization guide explains step-by-step the procedure of developing a recrystallization process. It explains what information is required at each stage of recrystallization and outlines how to control critical process parameter

Solubility and Metastable Zone Width (mzw) Determination

Solubility curves are commonly used to illustrate the relationship between solubility, temperature, and solvent type. By plotting temperature vs. solubility, scientists can create the framework needed to develop the desired crystallization process. Once an appropriate solvent is chosen, the solubility curve becomes a critical tool for the development of an effective crystallization process.

Tvorba jader a růst krystalů

Vědci a inženýři mají úplnou kontrolu nad celým procesem krystalizace díky možnosti přesného stanovení úrovně přesycení v průběhu procesu. Přesycení je hnací silou při tvorbě jader a růstu během krystalizace a rozhoduje o výsledné distribuci velikosti krystalů.

Measure Crystal Size Distribution

In-process probe-based technologies are applied to track particle size and shape changes at full concentration with no dilution or extraction necessary. By tracking the rate and degree of change to particles and crystals in real time, the correct process parameters for crystallization performance can be optimized.

Crystallization Seeding Protocol

Seeding is one of the most critical steps in optimizing crystallization behavior. When designing a seeding strategy, parameters such as: seed size, seed loading (mass), and seed addition temperature must be considered. These parameters are generally optimized based on process kinetics and the desired final particle properties, and must remain consistent during scale-up and technology transfer.

Particle Engineering and Wet Milling

Milling of dry powders can cause significant yield losses and can generate dust, creating health and safety hazards. In response to this, wet milling produces particles with a specifically designed size distribution. It is now common to employ high shear wet milling to break large primary crystals and agglomerates into fine particles.

Anti-Solvent Addition on Supersaturation

In an antisolvent crystallization, the solvent addition rate, addition location and mixing impact local supersaturation in a vessel or pipeline. Scientists and engineers modify crystal size and count by adjusting antisolvent addition protocol and the level of supersaturation.

Temperature Effects Crystallization Size and Shape

Crystallization kinetics are characterized in terms of two dominant processes, nucleation kinetics and growth kinetics, occurring during crystallization from solution. Nucleation kinetics describe the rate of formation of a stable nuclei. Growth kinetics define the rate at which a stable nuclei grows to a macroscopic crystal. Advanced techniques offer temperature control to modify supersaturation and crystal size and shape.

Temperature Effects Crystallization Size and Shape

Changing the scale or mixing conditions in a crystallizer can directly impact the kinetics of the crystallization process and the final crystal size. Heat and mass transfer effects are important to consider for cooling and antisolvent systems respectively, where temperature or concentration gradients can produce inhomogeneity in the prevailing level of supersaturation.

Chemical Process Development & Scale-Up

Design Robust and Sustainable Chemical Processes For Faster Transfer To Pilot Plant and Production

Chemical Reaction Kinetics Studies

In situ chemical reaction kinetics studies provide an improved understanding of reaction mechanism and pathway by providing concentration dependences of reacting components in real-time. Continuous data over the course of a reaction allows for the calculation of rate laws with fewer experiments due to the comprehensive nature of the data.  Reaction Progression Kinetics Analysis (RPKA) uses in situ data under synthetically relevant concentrations and captures information throughout the whole experiment ensuring that the complete reaction behavior can be accurately described.

Polymorphism Identification and Control

Polymorphism is a common phenomenon with many crystalline solids in the pharmaceutical and fine chemical industry. Scientists deliberately crystallize a desired polymorph to improve isolation properties, help overcome downstream process challenges, increase bioavailability or to prevent patent conflicts. Identifying polymorphic and morphological transformations in-situ and in real time eliminates unexpected process upset, out of specification product and costly reprocessing of material.

Publikace ke stažení

Publications on Crystallization Kinetics

White Papers

Pochopte krystalizaci pomocí in situ mikroskopie
Dynamické mechanismy představují klíč k pochopení krystalizačních procesů. Nyní je lze pozorovat pomocí in situ mikroskopie. V naší nové Bílé knize se...
Effective Crystallization Process Development
The quality of a crystallization process greatly influences the quality of the final product. Our new white paper introduces you to the fundamentals o...
Strategie pro řízenou distribuci velikosti krystalů
Tato bílá kniha je věnována strategiím optimalizace distribuce velikosti krystalů při vývoji procesů a výrobě.
Kvalitnější průmyslová krystalizace
Průmyslová krystalizace je důležitý separační a čisticí krok v chemickém průmyslu. Bílá kniha je věnována možnostem využití technologie in-line měření...
Seeding a Crystallization Process
Seeding is a key step in optimizing a crystallization process, ensuring a consistent filtration rate, yield, polymorphic form and particle size distri...
Scale-up of Batch Crystallization From Lab to Plant
Real-time monitoring of crystallization is shown to provide benefits leading to improved methods for process development, optimization and scale-up. T...
Best Practices For Crystallization Development
This white paper demonstrates the methodology chemists use to optimize critical crystallization parameters such as: Temperature profile Addition rates...
Bílá kniha na téma in-line charakterizace velikosti částic
Tradiční měření velikosti částic a kapek vyžaduje odběr vzorků s následným měřením mimo výrobní linku. V naší nové bílé knize se dočtete, jak lépe poc...

Webinars

Designing Continuous Crystallization Platforms
This webinar describes an investigation into the characterization, design and operation of continuous crystallization. Robust crystallization process...
Eliminating Micronization Using Fine Particle Crystallization
Crystal engineering is applied when the crystal size distribution is too large to meet downstream specifications. By designing the crystallization to...
Calibration Free Supersaturation Assessment
The quantitative use of in situ ATR-FTIR for real time supersaturation assessment has been extremely well defined within the literature. However, thes...
metastable zone width (MSZW) crystallization
The webinar focuses on a semi-quantitative method for the optimization and scale-up of hydrodynamically limited anti-solvent crystallization process....
Improving Crystallization and Precipitation
This webinar introduces case studies and highlights best practices used to overcome crystallization and precipitation challenges. The focus will be on...

Application Notes

In-Process Characterization of Antisolvent Crystallization
Ensure fast and efficient scale-up by optimizing crystallization early in development. Target particle size specifications to speed up downstream proc...
Polymorph and Pseudo-polymorph Transition in-process monitoring of habit change
Improve purity by ensuring total polymorphic form conversion. Enhance process robustness by monitoring crystallization processes in real time. Charact...

Citations

Crystallization and Precipitation Citation List
Crystallization and precipitation citation list and publications

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