Flow-Xl: a new facility for the analysis of crystallization in flow systems

Area of Science:

• Materials Science
• Chemical Engineering
• Physical Chemistry

Background:

• Understanding crystallization processes is crucial for controlling material properties.
• In situ characterization provides insights into nucleation and growth dynamics.
• Current methods often lack the temporal resolution to capture rapid crystallization events.

Purpose of the Study:

• To present a novel laboratory facility (Flow-Xl) for time-resolved in situ characterization of crystallization.
• To demonstrate the combined use of X-ray diffraction and Raman spectroscopy for monitoring crystallization.
• To analyze crystallization mechanisms and kinetics in real-time.

Main Methods:

• Development and implementation of the Flow-Xl facility integrating X-ray diffraction and Raman spectroscopy.
• Utilizing segmented and continuous flow platforms for sample handling.
• Acquisition of time-resolved data at second-scale resolution.

Main Results:

• The Flow-Xl facility enables high-resolution, time-resolved in situ structural and molecular data collection.
• Commissioning experiments confirmed the sensitivity of the instruments for flow samples.
• A case study on sodium sulfate crystallization demonstrated the ability to track kinetics and mechanisms.

Conclusions:

• The Flow-Xl facility offers a powerful tool for laboratory-based analysis of crystallization processes.
• Combined diffraction and spectroscopy provide comprehensive insights into crystallization mechanisms and kinetics.
• This approach advances the understanding of solid form development in solution.