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Instruments / Technical Area	Publication Details	Published	Actions
I14-Hard X-ray Nanoprobe	Nanoscale chemical imaging of nanoparticles under real‐world wastewater treatment conditions Miguel A. Gomez-Gonzalez , Mohamed A. Koronfel , Huw Pullin , Julia E. Parker , Paul D. Quinn , Maria D. Inverno , Thomas B. Scott , Fang Xie , Nikolaos Voulvoulis , Marian L. Yallop , Mary P. Ryan , Alexandra E. Porter Advanced Sustainable Systems 45 DOI: 10.1002/adsu.202100023 Diamond Proposal Number(s): [17784] Show Abstract ▼ Abstract: Understanding nanomaterial transformations within wastewater treatment plants is an important step to better predict their potential impact on the environment. Here, spatially resolved, in situ nano‐X‐ray fluorescence microscopy is applied to directly observe nanometer‐scale dissolution, morphological, and chemical evolution of individual and aggregated ZnO nanorods in complex “real‐world” conditions: influent water and primary sludge collected from a municipal wastewater system. A complete transformation of isolated ZnO nanorods into ZnS occurs after only 1 hour in influent water, but larger aggregates of the ZnO nanorods transform only partially, with small contributions of ZnS and Zn‐phosphate (Zn3(PO4)2) species, after 3 hours. Transformation of aggregates of the ZnO nanorods toward mixed ZnS, Zn adsorbed to Fe‐oxyhydroxides, and a large contribution of Zn3(PO4)2 phases are observed during their incubation in primary sludge for 3 hours. Discrete, isolated ZnO regions are imaged with unprecedented spatial resolution, revealing their incipient transformation toward Zn3(PO4)2. Passivation by transformation(s) into mixtures of less soluble phases may influence the subsequent bioreactivity of these nanomaterials. This work emphasizes the importance of imaging the nanoscale chemistry of mixtures of nanoparticles in highly complex, heterogeneous semi‐solid matrices for improved prediction of their impacts on treatment processes, and potential environmental toxicity following release.	May 2021
I14-Hard X-ray Nanoprobe	Spatially resolved dissolution and speciation changes of ZnO nanorods during short-term in situ incubation in a simulated wastewater environment Miguel A. Gomez-Gonzalez , Mohamed A. Koronfel , Angela Erin Goode , Maryam Al-Ejji , Nikolaos Voulvoulis , Julia E. Parker , Paul D. Quinn , Thomas Bligh Scott , Fang Xie , Marian L. Yallop , Alexandra E. Porter , Mary P. Ryan Acs Nano DOI: 10.1021/acsnano.9b02866 Diamond Proposal Number(s): [17784] Show Abstract ▼ Abstract: Zinc oxide engineered nanomaterials (ZnO ENMs) are used in a variety of applications worldwide due to their optoelectronic and antibacterial properties with potential contaminant risk to the environment following their disposal. One of the main potential pathways for ZnO nanomaterials to reach the environment is via urban wastewater treatment plants. So far there is no technique that can provide spatiotemporal nanoscale information about the rates and mechanisms by which the individual nanoparticles transform. Fundamental knowledge of how the surface chemistry of individual particles change, and the heterogeneity of transformations within the system, will reveal the critical physicochemical properties determining environmental damage and deactivation. We applied a methodology based on spatially resolved in situ X-ray fluorescence microscopy (XFM), allowing observation of real-time dissolution and morphological and chemical evolution of synthetic template-grown ZnO nanorods (∼725 nm length, ∼140 nm diameter). Core–shell ZnO-ZnS nanostructures were formed rapidly within 1 h, and significant amounts of ZnS species were generated, with a corresponding depletion of ZnO after 3 h. Diffuse nanoparticles of ZnS, Zn3(PO4)2, and Zn adsorbed to Fe-oxyhydroxides were also imaged in some nonsterically impeded regions after 3 h. The formation of diffuse nanoparticles was affected by ongoing ZnO dissolution (quantified by inductively coupled plasma mass spectrometry) and the humic acid content in the simulated sludge. Complementary ex situ X-ray absorption spectroscopy and scanning electron microscopy confirmed a significant decrease in the ZnO contribution over time. Application of time-resolved XFM enables predictions about the rates at which ZnO nanomaterials transform during their first stages of the wastewater treatment process.	Sep 2019

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