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A Vibrational Spectroscopic Study of the Phosphate Mineral Minyulite Kal2(OH,F)(PO4)2.4(H2O) and in Comparison with Wardite

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A Vibrational Spectroscopic Study of the Phosphate Mineral Minyulite Kal2(OH,F)(PO4)2.4(H2O) and in Comparison with Wardite This may be the author’s version of a work that was submitted/accepted for publication in the following source: Frost, Ray, Lopez, Andres, Xi, Yunfei, Cardoso, Luiz Henrique, & Scholz, Ricardo (2014) A vibrational spectroscopic study of the phosphate mineral minyulite KAl2(OH,F)(PO4)2.4(H2O) and in comparison with wardite. Spectrochimica Acta - Part A: Molecular and Biomolecular Spectroscopy, 124, pp. 34-39. This file was downloaded from: https://eprints.qut.edu.au/66530/ c Copyright 2013 Elsevier B.V. NOTICE: this is the author?s version of a work that was accepted for publication in Spec- trochimica Acta Part A: Molecular and Biomolecular Spectroscopy. Changes resulting from the publishing process, such as peer review, editing, corrections, structural formatting, and other quality control mechanisms may not be reflected in this document. Changes may have been made to this work since it was submitted for publication. A definitive version was subsequently published in Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, [Volume 124, 24 (April 2014)] DOI: 10.1016/j.saa.2013.12.039 License: Creative Commons: Attribution-Noncommercial-No Derivative Works 4.0 Notice: Please note that this document may not be the Version of Record (i.e. published version) of the work. Author manuscript versions (as Sub- mitted for peer review or as Accepted for publication after peer review) can be identified by an absence of publisher branding and/or typeset appear- ance. If there is any doubt, please refer to the published source. https://doi.org/10.1016/j.saa.2013.12.039 1 A vibrational spectroscopic study of the phosphate mineral minyulite 2 KAl2(OH,F)(PO4)2·4(H2O) and in comparison with wardite 3 4 Ray L. Frost,a• Andrés López,a Yunfei Xia, Luiz Henrique Cardosob and Ricardo 5 Scholzb 6 7 a School of Chemistry, Physics and Mechanical Engineering, Science and Engineering 8 Faculty, Queensland University of Technology, GPO Box 2434, Brisbane Queensland 9 4001, Australia. 10 11 b Geology Department, School of Mines, Federal University of Ouro Preto, Campus Morro 12 do Cruzeiro, Ouro Preto, MG, 35,400-00, Brazil. 13 14 ABSTRACT 15 Vibrational spectroscopy enables subtle details of the molecular structure of minyulite 16 KAl2(OH,F)(PO4)2·4(H2O). Single crystals of a pure phase from a Brazilian pegmatite were 17 used. Minyulite belongs to the orthorhombic crystal system. This indicates that it has three 18 axes of unequal length, yet all are perpendicular to each other. The infrared and Raman 19 spectroscopy were applied to compare the structure of minyulite with wardite. The reason for 20 the comparison is that both are Al containing phosphate minerals. -1 21 The Raman spectrum of minyulite shows an intense band at 1012 cm assigned to the ν1 3- 22 PO4 symmetric stretching vibrations. A series of low intensity Raman bands at 1047, 1077, -1 3- 23 1091 and 1105 cm are assigned to the ν3 PO4 antisymmetric stretching modes. The 24 Raman bands at 1136, 1155, 1176 and 1190 cm-1 are assigned to AlOH deformation modes. -1 3- 25 The infrared band at 1014 cm is ascribed to the PO4 ν1 symmetric stretching vibrational -1 3- 26 mode. The infrared bands at 1049, 1071, 1091 and 1123 cm are attributed to the PO4 ν3 27 antisymmetric stretching vibrations. The infrared bands at 1123, 1146 and 1157 cm-1 are 28 attributed to Al OH deformation modes. Raman bands at 575, 592, 606 and 628 cm-1 are 3- -1 29 assigned to the ν4 out of plane bending modes of the PO4 unit. In the 2600 to 3800 cm 30 spectral range, Raman bands for minyulite are found at 3661, 3669 and 3692 cm-1 are 31 assigned to AlOH/AlF stretching vibrations. Broad infrared bands are also found at 2904, 32 3105, 3307, 3453 and 3523 cm-1. Raman bands at 3225, 3324 cm-1 are assigned to water • Author to whom correspondence should be addressed ([email protected]) 1 33 stretching vibrations. A comparison is made with the vibrational spectra of wardite. Raman 34 spectroscopy complimented with infrared spectroscopy has enabled aspects of the structure of 35 minyulite to be ascertained and compared with that of other phosphate minerals. 36 37 Keywords: minyulite, wardite, phosphate, hydroxyl, Raman spectroscopy, infrared 38 2 39 1. Introduction 40 Minyulite [1] is a rare phosphate mineral with a chemical formula of 41 KAl2(OH,F)(PO4)2·4(H2O). It occurs as groups of radiating fine fibrous crystals within rock 42 cracks of weathered glauconitic phosphatic ironstone [2]. It was first described in 1933 for an 43 occurrence in Western Australia and named after the type locality Minyulo Well in Western 44 Australia [1]. Minyulite is considered as a secondary phosphate since it is formed by the 45 alteration of a primary phosphate [2]. Primary phosphates are phosphates that are mined on a 46 large scale for example ‘super phosphate’ of calcium phosphate. The mineral minyulite 47 occurs in association with other phosphate minerals including dufrenite, apatite, fluellite, 48 wavellite, variscite and leucophosphate all of which are secondary phosphate minerals [3]. 49 The mineral is known from many locations worldwide [4-7]. The mineral is found in many 50 Australian localities including from near Minyulo Well, Dandarragan, Western Australia; in 51 Wait’s quarry and Oliver’s quarry, near Noarlunga, 32 km south of Adelaide; in the Moculta 52 phosphate quarry, northeast of Angaston, and from the St. John’s quarry, seven km southeast 53 of Kapunda, Mount Lofty Ranges, South Australia; at Wolfdene, near Beenleigh, Brisbane, 54 Queensland.The mineral can be found in the underlying phosphatized rock zone of 55 ornithogenic soil. Minyulite is not found in abundance, it can be found in the sea shore of the 56 maritime Arctic and Antarctic [8, 9]. The mineral minyulite is known from a wide range of 57 deposits world-wide for example in Italy and in the USA. A comparison may be made with 58 the mineral wardite NaAl3(PO4)2(OH)4·2(H2O). 59 Minyulite belongs to the orthorhombic crystal system [10, 11]. This indicates that it has three 60 axes of unequal length, yet all are perpendicular to each other. The Space Group is Pba2. a = 61 9.337(5) b = 9.740(5) c = 5.522(3) and Z = 2. The mineral wardite is unusual in that it 62 belongs to a unique symmetry class, namely the tetragonal-trapezohedral group [12]. This 63 class has only a 4 fold rotational axis and two 2 fold rotational axes and nothing else. Crystals 64 of wardite show the lower symmetry by displaying squashed pseudo-octahedrons with 65 striated faces. 66 The crystal structures of natural wardite and of the isomorphous cyrilovite have been solved 67 [12, 13]. The structure of cyrilovite was further refined by Cooper et al. The cell dimensions 68 are Space Group: P41212 or P43212. a = 7.03(1) Å, c = 19.04(1)Å, Z = 4. The structures 69 contain layers of two kinds of corner-linked –OH bridged MO6 octahedra (M =Al, Fe), 70 stacked along the tetragonal C-axis in a four-layer sequence and linked by PO4 groups. 3 71 Within a layer, e.g. around the (001) plane, two independent pairs of symmetry-correlated – 72 OH groups are arranged in the equatorial pseudo-planes of one kind of MO6 octahedra [12, 73 13]. 74 Raman spectroscopy has proven very useful for the study of minerals [14-20]. Indeed, 75 Raman spectroscopy has proven most useful for the study of diagenetically related minerals 76 where isomorphic substitution may occur as with wardite, cyrilovite and minyulite, as often 77 occurs with minerals containing phosphate groups. This paper is a part of systematic studies 78 of vibrational spectra of minerals of secondary origin. The objective of this research is to 79 report the Raman and infrared spectra of minyulite and to relate the spectra to the molecular 80 structure of the mineral. 81 2. Experimental 82 2.1 Samples description and preparation 83 The minyulite sample studied in this work was collected from Minyulo Well, Australia. The 84 formula corresponds to (K0.82,Ca0.05,Na0.03)(Al2.04,Fe0.08)(PO4)2[F0.55(OH)0.45] ∙4H2O. The 85 sample was incorporated to the collection of the Geology Department of the Federal 86 University of Ouro Preto, Minas Gerais, Brazil, with sample code SAB-193. The sample was 87 gently crushed and the associated minerals were removed under a stereomicroscope Leica 88 MZ4. The minyulite sample was phase analyzed by X-ray diffraction. Scanning electron 89 microscopy (SEM) in the EDS mode was applied to support the mineral characterization. 90 91 The mineral wardite was supplied by the Mineralogical Research Company. Wardite 92 originated from Lavra Da Ilha, Minas Gerais, Brazil. Details of this mineral have been 93 published (page 643) [21]. 94 95 2.2 Raman spectroscopy 96 Crystals of minyulite were placed on a polished metal surface on the stage of an Olympus 97 BHSM microscope, which is equipped with 10x, 20x, and 50x objectives. The microscope is 98 part of a Renishaw 1000 Raman microscope system, which also includes a monochromator, a 99 filter system and a CCD detector (1024 pixels). The Raman spectra were excited by a 100 Spectra-Physics model 127 He-Ne laser producing highly polarised light at 633 nm and 101 collected at a nominal resolution of 2 cm-1 and a precision of ± 1 cm-1 in the range between 102 200 and 4000 cm-1. Some of these mineral fluoresced badly at 633 nm; as a consequence 4 103 other laser excitation wavelengths were used especially the 785 nm laser.
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