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Systematic Raman Spectroscopic Study of the Isomorphy Between the Arsenate Minerals Roselite, Wendwilsonite, Zincroselite, Brandtite, and Rruffite

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Systematic Raman Spectroscopic Study of the Isomorphy Between the Arsenate Minerals Roselite, Wendwilsonite, Zincroselite, Brandtite, and Rruffite Author Accepted Manuscript DOI: 10.1177/0003702820984254 Systematic Raman Spectroscopic Study of the Isomorphy Between the Arsenate Minerals Roselite, Wendwilsonite, Zincroselite, Brandtite, and Rruffite. Journal: Applied Spectroscopy Manuscript ID ASP-20-0302.R1 ManuscriptPeer Type: Submitted Review Manuscript Version Date Submitted by the 25-Nov-2020 Author: Complete List of Authors: Kloprogge, J.; University of the Philippines Visayas, Chemistry; The University of Queensland - Saint Lucia Campus, School of Earth and Environmental Sciences arsenate, roselite group, roselite, zincroselite, brandtite, wendwilsonite, Manuscript Keywords: rruffite, Raman spectroscopy In nature a wide variety of minerals are known with the general formula X2M(TO4)2·2(H2O) and an important group is formed by minerals with T = As. Most of these occur as minor or trace minerals in environments such as hydrothermal alterations of primary sulfides and arsenides. X- ray Photoelectron Spectroscopy (XPS) and Raman microspectroscopy have been utilized to study the chemistry and crystal structure of the roselite subgroup minerals, Ca2M(AsO4)2·2H2O (with M = Co, Mg, Mn, Zn, and Cu). The arsenate AsO4 stretching region exhibited minor differences between the roselite subgroup minerals, which can be explained by the ionic radius of the cation substituting on the M position in the structure. Multiple AsO4 antisymmetric stretching vibrations were found, pointing to a tetrahedral symmetry reduction. Similar observations were made for the corresponding bending modes. Bands around 450 cm-1 were attributed to ν4 bending modes. Several bands in Abstract: the 300–350cm-1 region attributed to ν2 bending modes also provide evidence of symmetry reduction of the AsO4 anion. Two broad bands for roselite were found around 3330 and 3120 cm-1 and were attributed to the OH stretching bands of crystal water. These bands are accompanied by two bands around 1700 and 1610 cm-1 attributed to the corresponding OH-bending modes. In conclusion, both XPS and Raman spectroscopy have been shown here to be valuable non-destructive analytical tools to characterize these secondary arsenate minerals. X-ray Photoelectron Spectroscopy and Raman microspectroscopy allow the chemistry and molecular structure of the roselite subgroup minerals to be studied in a non-destructive way. The minerals in the roselite subgroup are easily distinguished based on their chemical composition as determined by XPS. As expected for minerals with the same crystal structure, similarities exist in the Raman spectra, sufficient differences exist to be able to identify these minerals. Applied Spectroscopy Page 1 of 36 Author Accepted Manuscript 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 Peer Review Version 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 Applied Spectroscopy Author Accepted Manuscript Page 2 of 36 1 2 3 4 Systematic Raman Spectroscopic Study of the Isomorphy Between the 5 6 Arsenate Minerals Roselite, Wendwilsonite, Zincroselite, Brandtite, and 7 8 Rruffite. 9 10 11 J. Theo Kloprogge1,2* 12 13 1 Department of Chemistry, College of Arts and Sciences, University of the Philippines Visayas, 14 15 Miag-ao, Iloilo 5023, Philippines 16 2 School of Earth and Environmental Sciences, The University of Queensland, Brisbane, Qld 17 Peer Review Version 18 4072, Australia 19 20 21 *Corresponding author email: 22 23 Email: [email protected] 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 1 59 60 Applied Spectroscopy Page 3 of 36 Author Accepted Manuscript 1 2 3 ABSTRACT 4 5 In nature numerous minerals are known with the general formula X2M(TO4)2·2(H2O) and an 6 7 important group is formed by minerals with T = As. Most of these occur as minor or trace 8 minerals in environments such as hydrothermal alterations of primary sulfides and arsenides. X- 9 10 ray photoelectron spectroscopy and Raman spectroscopy have been utilized to study the 11 12 chemistry and crystal structure of the roselite subgroup minerals, Ca2M(AsO4)2·2H2O (with M = 13 14 Co, Mg, Mn, Zn, and Cu). The AsO4 stretching region exhibited minor differences between the 15 roselite subgroup minerals, which can be explained by the ionic radius of the cation substituting 16 Peer Review Version 17 on the M position in the structure. Multiple AsO4 antisymmetric stretching and bending modes 18 19 were found, pointing to a tetrahedral symmetry reduction. Bands around 450 cm-–1 were 20 -–1 21 attributed to ν4 bending modes. Several bands in the 300–350 cm region attributed to ν2 22 bending modes also provide evidence of symmetry reduction of the AsO anion. Two broad 23 4 24 bands for roselite were found around 3330 and 3120 cm-–1 and were attributed to the OH 25 26 stretching bands of crystal water. These bands are accompanied by two bands around 1700 and 27 -–1 28 1610 cm attributed to the corresponding OH-bending modes. In conclusion, both XPS and 29 Raman spectroscopy are valuable non-destructive analytical tools to characterize these secondary 30 31 arsenate minerals. X-ray Photoelectron Spectroscopy and Raman microspectroscopy allow the 32 33 chemistry and molecular structure of the roselite group minerals to be studied in a non- 34 destructive way. The minerals in the roselite subgroup are easily distinguished based on their 35 36 chemical composition as determined by XPS. As expected for minerals with the same crystal 37 38 structure, similarities exist in the Raman spectra, sufficient differences exist to be able to identify 39 40 these minerals. 41 Keywords: arsenateArsenate;, roselite group;, roselite;, wendwilsonite;, zincroselite;, brandtite;, 42 43 rruffite;, Raman spectroscopy;, isomorphy 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 2 59 60 Applied Spectroscopy Author Accepted Manuscript Page 4 of 36 1 2 3 4 5 INTRODUCTION 6 7 In nature a wide variety of minerals are known with the general formula X2M(TO4)2.2(H2O) and 8 an important group is formed by minerals with T = As.1 Most of these are found as minor or 9 10 trace minerals in environments such as hydrothermal alterations of primary sulfides and 11 12 arsenides arsenides.2, 3. One of the groups that fit this profile is the roselite group, consisting of 13 14 the minerals roselite, wendwilsonite, zincroselite, brandtite and rruffite, which are all arsenates 15 and the isostructural hydrated sulfate kröhnkite. Within this group in all cases X is Ca, except for 16 Peer Review Version 17 kröhnkite where it is Na, but M can be a variety of metals, e.g. Co, Mg, Mn, Zn, and Cu. 18 19 All minerals in the roselite subgroup crystallize in the monoclinic system with space group 20 21 P21/c. The As atoms are in a regular tetrahedral coordination with four O atoms. The M-site 22 metals are typically divalent and are in an octahedral coordination with four O atoms and two 23 24 (H2O) groups. The Ca atoms are positioned in an irregular [8]-coordinated polyhedron of seven 25 2 26 O atoms and one (H2O) group. The characteristic building block is an infinite chain parallel to 27 the c-axis of octahedral and tetrahedra with composition [M(TO )(H O) ], in which isolated MO 28 4 2 2 6 29 octahedra are connected by corner sharing with TO4 tetrahedra (Fig. 1). This type of chain is 30 31 known as the kröhnkite-type chain, since it was first discovered in kröhnkite.4, 5 32 33 Roselite was originally named in honourhonor of German mineralogist Gustav Rose (18 34 March 18, 1798 Berlin, Germany –15 July 15, 1873 in Berlin, Germany]), Professor of 35 36 Mineralogy, University of Berlin, as an orthorhombic arsenate of lime and cobalt. 6. 37 38 Approximately fifty years 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 3 59 60 Applied Spectroscopy Page 5 of 36 Author Accepted Manuscript 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 Peer Review Version 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 Figure 1 Crystal structures of roselite, zincroselite, brandtite, wendwilsonite and rruffite 45 46 47 later, Schrauf determined that roselite was not orthorhombic, but had pseudo-orthorhombic 48 49 triclinic elements, that the crystals were lamellar twinned on as many as five of the six elements 50 51 of pseudo-symmetry of the chosen lattice.7-–9 It was Peacock though who finally showed 52 10 53 conclusively that roselite is monoclinic. Roselite has now definitively been determined as 54 belonging to the monoclinic system with point group 2/m (space group P21/c), a = 5.801(1), b = 55 56 57 58 4 59 60 Applied Spectroscopy Author Accepted Manuscript Page 6 of 36 1 2 3 12.898(3), c = 5.617(1), β = 107°42(2)’, Z =2. Crystals tend to be elongated along [100], and] 4 5 and are commonly twinned on {100} with {100} as composition plane.3, 1,11, 1,12 6 7 Wendwilsonite is the Mg-member of the roselite group and exists as a continuous series 8 with roselite. It is pale to intense pink, may even be red and colour zoning is commonly 9 10 observed.3, 1,13 Kolitsch and Fleck 11 reported on the exact crystal structure as part of their 11 12 comprehensive study of minerals and synthetic materials with kröhnkite-type chains.
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