High-temperature study of basic ferric sulfate, FeOHSO 4
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ORIGINAL PAPER
High‑temperature study of basic ferric sulfate, FeOHSO4 Gennaro Ventruti1 · Giancarlo Della Ventura2,3 · Mario Alberto Gomez4 · Giancarlo Capitani5 · Marco Sbroscia2 · Armida Sodo2 Received: 12 June 2020 / Accepted: 13 September 2020 / Published online: 1 October 2020 © The Author(s) 2020
Abstract We report in this paper a new crystal-chemical study of synthetic basic ferric sulfate F eOHSO4. The structure solution performed by the Endeavour program, from new X-ray powder diffraction (XRPD) data, indicated that the correct space group of the monoclinic polytype of F eOHSO4 is C2/c. Selected Area Electron Diffraction (SAED) patterns are also consistent with this structure solution. The arrangement of Fe and S atoms, based on linear chains of F e3+ octahedra cross-linked by S O4 tetrahedra, corresponds to that of the order/disorder (OD) family. The positions of the hydrogen atoms were located based on DFT calculations. IR and Raman spectra are presented and discussed according to this new structure model. The decomposition of F eOHSO4 during heating was further investigated by means of variable temperature XRPD, thermogravimetry, and differential thermal analysis as well as IR and Raman spectroscopies. Keywords Sulfate · Crystal structure · Thermal stability · HT-FTIR · Raman
Introduction The basic iron hydroxyl sulfate, FeOHSO4, has attracted in the last decades significant attention in many research fields such as environmental science, catalysis, electrochemistry, mineralogy, and soil science (Cheng and Demopoulos 2004; Fleming 2010; Xu et al. 2010; Reddy et al. 2009). It is also known to form during the thermal decomposition of hydrates Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00269-020-01113-7) contains supplementary material, which is available to authorized users. * Gennaro Ventruti [email protected] 1
Dipartimento di Scienze della Terra e Geoambientali, Università di Bari, via Orabona, 4, 70125 Bari, Italy
2
Dipartimento di Scienze, Università Roma Tre, Largo S. Leonardo Murialdo 1, 00146 Rome, Italy
3
INFN-LNF, Frascati, Rome, Italy
4
Liaoning Engineering Research Center for Treatment and Recycling of Industrially Discharged Heavy Metals, Shenyang University of Chemical Technology, Shenyang 110142, China
5
Department of Earth and Environmental Sciences, University of Milano-Bicocca, Piazza della Scienza, 4, 20126 Milano, Italy
of Fe2+ sulfate (e.g., Swamy and Prasad 1981; Pelovski et al. 1996) and other secondary iron-sulfate minerals (e.g., Ventruti et al. 2014, 2016). The crystal structure FeOHSO4 was solved by Johansson (1962) in the orthorhombic space group Pnma and described as consisting of linear chains of Fe3+ octahedra cross-linked by SO4 tetrahedra. More recently, Ventruti et al. (2005) demonstrated, based on the OD theory, that this compound may crystallize under two different polytypes. The first corresponds to the orthorhombic polytype reported by Johansson (1962). The s
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