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Journal of Synchrotron Radiation
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Journal of Synchrotron Radiation
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A flow-through reaction cell forin situX-ray diffraction and absorption studies of heterogeneous powder–liquid reactions and phase transformations

Authors: Ferrer Escorihuela, Pilar; Da Silva González, Jesús Iván; Rubio Zuazo, Juan; Fernández Alfonso, María Belén Aurora; Trobajo Fernández, María del Camino; Khaynakov, Sergiy; Rodríguez García, José; +2 Authors

A flow-through reaction cell forin situX-ray diffraction and absorption studies of heterogeneous powder–liquid reactions and phase transformations

Abstract

A portable powder–liquid high-corrosion-resistant reaction cell has been designed to followin situreactions by X-ray powder diffraction (XRD) and X-ray absorption spectroscopy (XAS) techniques. The cell has been conceived to be mounted on the experimental stations for diffraction and absorption of the Spanish CRG SpLine-BM25 beamline at the European Synchrotron Radiation Facility. Powder reactants and/or products are kept at a fixed position in a vertical geometry in the X-ray pathway by a porous membrane, under forced liquid reflux circulation. Owing to the short pathway of the X-ray beam through the cell, XRD and XAS measurements can be carried out in transmission configuration/mode. In the case of the diffraction technique, data can be collected with either a point detector or a two-dimensional CCD detector, depending on specific experimental requirements in terms of space or time resolution. Crystallization processes, heterogeneous catalytic processes and several varieties of experiments can be followed by these techniques with this cell. Two experiments were carried out to demonstrate the cell feasibility: the phase transformations of layered titanium phosphates in boiling aqueous solutions of phosphoric acid, and the reaction of copper carbonate and L-isoleucine amino acid powders in boiling aqueous solution. In this last case the shrinking of the solid reactants and the formation of Cu(isoleucine)2is observed. The crystallization processes and several phase transitions have been observed during the experiments, as well as an unexpected reaction pathway.

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selected citations
These citations are derived from selected sources.
This is an alternative to the "Influence" indicator, which also reflects the overall/total impact of an article in the research community at large, based on the underlying citation network (diachronically).
BIP!Citations provided by BIP!
popularity
This indicator reflects the "current" impact/attention (the "hype") of an article in the research community at large, based on the underlying citation network.
BIP!Popularity provided by BIP!
influence
This indicator reflects the overall/total impact of an article in the research community at large, based on the underlying citation network (diachronically).
BIP!Influence provided by BIP!
impulse
This indicator reflects the initial momentum of an article directly after its publication, based on the underlying citation network.
BIP!Impulse provided by BIP!
views
OpenAIRE UsageCountsViews provided by UsageCounts
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