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Droplet-based in situ X-ray absorption spectroscopy cell for studying crystallization processes at the tender X-ray energy range

The understanding of nucleation and crystallization is fundamental in science and technology. In solution, these processes are complex involving multiple transformations from ions and ion pairs through amorphous intermediates to multiple crystalline phases. X-ray absorption spectroscopy (XAS), which...

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Autores principales: Xto, Jacinta, Wetter, Reto, Borca, Camelia N., Frieh, Christophe, van Bokhoven, Jeroen A., Huthwelker, Thomas
Formato: Online Artículo Texto
Lenguaje:English
Publicado: The Royal Society of Chemistry 2019
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9073857/
https://www.ncbi.nlm.nih.gov/pubmed/35528920
http://dx.doi.org/10.1039/c9ra06084g
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author Xto, Jacinta
Wetter, Reto
Borca, Camelia N.
Frieh, Christophe
van Bokhoven, Jeroen A.
Huthwelker, Thomas
author_facet Xto, Jacinta
Wetter, Reto
Borca, Camelia N.
Frieh, Christophe
van Bokhoven, Jeroen A.
Huthwelker, Thomas
author_sort Xto, Jacinta
collection PubMed
description The understanding of nucleation and crystallization is fundamental in science and technology. In solution, these processes are complex involving multiple transformations from ions and ion pairs through amorphous intermediates to multiple crystalline phases. X-ray absorption spectroscopy (XAS), which is sensitive to liquid, amorphous and crystalline phases offers prospects of demystifying these processes. However, for low Z elements the use of in situ X-ray absorption spectroscopy requires the tender X-ray range, which is often limited by vacuum requirements thereby complicating these measurements. To overcome these challenges, we developed a versatile and user-friendly droplet-based in situ X-ray absorption spectroscopy cell for studying crystallization processes. Time-resolved in situ experiments under ambient conditions are carried out in the cell whilst the cell is mounted in the vacuum chamber of a tender X-ray beamline. By following changes in the Ca K-edge X-ray absorption near edge structure (XANES), we captured in situ the intermediate phases involved during calcium carbonate crystallization from aqueous solutions. In addition, through linear combination fitting it was possible to qualitatively observe the evolution of each phase during the reaction demonstrating the potential of the cell in studying complex multiphase chemical processes.
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spelling pubmed-90738572022-05-06 Droplet-based in situ X-ray absorption spectroscopy cell for studying crystallization processes at the tender X-ray energy range Xto, Jacinta Wetter, Reto Borca, Camelia N. Frieh, Christophe van Bokhoven, Jeroen A. Huthwelker, Thomas RSC Adv Chemistry The understanding of nucleation and crystallization is fundamental in science and technology. In solution, these processes are complex involving multiple transformations from ions and ion pairs through amorphous intermediates to multiple crystalline phases. X-ray absorption spectroscopy (XAS), which is sensitive to liquid, amorphous and crystalline phases offers prospects of demystifying these processes. However, for low Z elements the use of in situ X-ray absorption spectroscopy requires the tender X-ray range, which is often limited by vacuum requirements thereby complicating these measurements. To overcome these challenges, we developed a versatile and user-friendly droplet-based in situ X-ray absorption spectroscopy cell for studying crystallization processes. Time-resolved in situ experiments under ambient conditions are carried out in the cell whilst the cell is mounted in the vacuum chamber of a tender X-ray beamline. By following changes in the Ca K-edge X-ray absorption near edge structure (XANES), we captured in situ the intermediate phases involved during calcium carbonate crystallization from aqueous solutions. In addition, through linear combination fitting it was possible to qualitatively observe the evolution of each phase during the reaction demonstrating the potential of the cell in studying complex multiphase chemical processes. The Royal Society of Chemistry 2019-10-24 /pmc/articles/PMC9073857/ /pubmed/35528920 http://dx.doi.org/10.1039/c9ra06084g Text en This journal is © The Royal Society of Chemistry https://creativecommons.org/licenses/by-nc/3.0/
spellingShingle Chemistry
Xto, Jacinta
Wetter, Reto
Borca, Camelia N.
Frieh, Christophe
van Bokhoven, Jeroen A.
Huthwelker, Thomas
Droplet-based in situ X-ray absorption spectroscopy cell for studying crystallization processes at the tender X-ray energy range
title Droplet-based in situ X-ray absorption spectroscopy cell for studying crystallization processes at the tender X-ray energy range
title_full Droplet-based in situ X-ray absorption spectroscopy cell for studying crystallization processes at the tender X-ray energy range
title_fullStr Droplet-based in situ X-ray absorption spectroscopy cell for studying crystallization processes at the tender X-ray energy range
title_full_unstemmed Droplet-based in situ X-ray absorption spectroscopy cell for studying crystallization processes at the tender X-ray energy range
title_short Droplet-based in situ X-ray absorption spectroscopy cell for studying crystallization processes at the tender X-ray energy range
title_sort droplet-based in situ x-ray absorption spectroscopy cell for studying crystallization processes at the tender x-ray energy range
topic Chemistry
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9073857/
https://www.ncbi.nlm.nih.gov/pubmed/35528920
http://dx.doi.org/10.1039/c9ra06084g
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