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Título: | Evidence for liquid-liquid phase separation during the early stages of Mg-struvite formation |
Autor: | Karafiludis, Stephanos; Scoppola, Ernesto; Wolf, Stephan E.; Kochovski, Zdravko; Matzdorff, David; Van Driessche, Alexander E. S.; Hövelmann, Jörn; Emmerling, Franziska; Stawski, Tomasz M. | Palabras clave: | Crystallization High resolution transmission electron microscopy Nitrogen compounds Phase separation Precipitation (chemical) X ray scattering Amorphous precursors Aqueous media Engineered environments Liquid-liquid phase separation Multisteps Scattering data Situ x-ray scatterings Struvite formation Struvites Time-resolved Magnesium compounds |
Fecha de publicación: | 7-oct-2023 | Editor: | American Institute of Physics | Citación: | Journal of Chemical Physics 159: 134503 (2023) | Resumen: | The precipitation of struvite, a magnesium ammonium phosphate hexahydrate (MgNHPO · 6HO) mineral, from wastewater is a promising method for recovering phosphorous. While this process is commonly used in engineered environments, our understanding of the underlying mechanisms responsible for the formation of struvite crystals remains limited. Specifically, indirect evidence suggests the involvement of an amorphous precursor and the occurrence of multi-step processes in struvite formation, which would indicate non-classical paths of nucleation and crystallization. In this study, we use synchrotron-based in situ x-ray scattering complemented by cryogenic transmission electron microscopy to obtain new insights from the earliest stages of struvite formation. The holistic scattering data captured the structure of an entire assembly in a time-resolved manner. The structural features comprise the aqueous medium, the growing struvite crystals, and any potential heterogeneities or complex entities. By analysing the scattering data, we found that the onset of crystallization causes a perturbation in the structure of the surrounding aqueous medium. This perturbation is characterized by the occurrence and evolution of Ornstein-Zernike fluctuations on a scale of about 1 nm, suggesting a non-classical nature of the system. We interpret this phenomenon as a liquid-liquid phase separation, which gives rise to the formation of the amorphous precursor phase preceding actual crystal growth of struvite. Our microscopy results confirm that the formation of Mg-struvite includes a short-lived amorphous phase, lasting >10 s. | Versión del editor: | http://dx.doi.org/10.1063/5.0166278 | URI: | http://hdl.handle.net/10261/343678 | Identificadores: | doi: 10.1063/5.0166278 issn: 1089-7690 |
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