Online Monitoring of the Concentrations of Amorphous and Crystalline Mesoscopic Species Present in Solution


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Date

2022-08-03

Publication Type

Journal Article

ETH Bibliography

yes

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Abstract

Despite the growing evidence for the existence of amorphous mesoscopic species in a solution and their crucial roles in crystallization, there has been the lack of a suitable method to measure the time-resolved concentrations of amorphous and crystalline mesospecies in a lab-scale stirred reactor. This has limited experimental investigations to understand the kinetics of amorphous and crystalline mesospecies formation in stirred solutions and made it challenging to measure the crystal nucleation rate directly. Here, we used depolarized light sheet microscopy to achieve time-resolved measurements of amorphous and crystalline mesospecies concentrations in solutions at varying temperatures. After demonstrating that the concentration measurement method is reasonably accurate, precise, and sensitive, we utilized this method to examine mesospecies formation both in a mixture of two miscible liquids and in an undersaturated solution of DL-valine, thus revealing the importance of a temperature change in the formation of metastable and amorphous mesospecies as well as the reproducibility of the measurements. Moreover, we used the presented method to monitor both mesospecies formation and crystal nucleation in DL-valine solutions at four different levels of supersaturation, while achieving the direct measurement of the crystal nucleation rates in stirred solutions. Our results show that, as expected, the inherent variability in nucleation originating from its stochastic nature reduces with increasing supersaturation, and the dependence of the measured nucleation rate on supersaturation is in reasonable agreement with that predicted by the classical nucleation theory.

Publication status

published

Editor

Book title

Volume

22 (8)

Pages / Article No.

5071 - 5080

Publisher

American Chemical Society

Event

Edition / version

Methods

Software

Geographic location

Date collected

Date created

Subject

Crystals; Nanoparticles; Nucleation; Solution chemistry; Supersaturation

Organisational unit

03484 - Mazzotti, Marco (emeritus) / Mazzotti, Marco (emeritus) check_circle

Notes

Funding

788607 - Studying Secondary Nucleation for the Intensification of Continuous Crystallization (EC)

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