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A Vibrational Spectroscopic Study of the Phosphate Mineral Whiteite

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A Vibrational Spectroscopic Study of the Phosphate Mineral Whiteite Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 124 (2014) 243–248 Contents lists available at ScienceDirect Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy journal homepage: www.elsevier.com/locate/saa A vibrational spectroscopic study of the phosphate mineral ++ whiteite CaMn Mg2Al2(PO4)4(OH)2Á8(H2O) ⇑ Ray L. Frost a, , Ricardo Scholz b, Andrés López a, Yunfei Xi a a School of Chemistry, Physics and Mechanical Engineering, Science and Engineering Faculty, Queensland University of Technology, GPO Box 2434, Brisbane Queensland 4001, Australia b Geology Department, School of Mines, Federal University of Ouro Preto, Campus Morro do Cruzeiro, Ouro Preto, MG, 35,400-00, Brazil highlights graphical abstract Vibrational spectroscopy enables subtle details of the molecular structure of whiteite. Crystals of a pure phase from a Brazilian pegmatite were used. Raman and infrared bands are assigned to the vibrations of 3À PO4 . A comparison is made with the vibrational spectra of wardite. article info abstract Article history: Vibrational spectroscopy enables subtle details of the molecular structure of whiteite to be determined. Received 8 October 2013 Single crystals of a pure phase from a Brazilian pegmatite were used. The infrared and Raman spectros- Received in revised form 17 December 2013 copy were applied to compare the molecular structure of whiteite with that of other phosphate minerals. Accepted 10 January 2014 À1 3À The Raman spectrum of whiteite shows an intense band at 972 cm assigned to the m1 PO4 symmetric Available online 21 January 2014 À1 3À stretching vibrations. The low intensity Raman bands at 1076 and 1173 cm are assigned to the m3 PO4 antisymmetric stretching modes. The Raman bands at 1266, 1334 and 1368 cmÀ1 are assigned to AlOH Keywords: deformation modes. The infrared band at 967 cmÀ1 is ascribed to the PO3À m symmetric stretching vibra- Whiteite 4 1 tional mode. The infrared bands at 1024, 1072, 1089 and 1126 cmÀ1 are attributed to the PO3À anti- Jahnsite 4 m3 À1 Phosphate symmetric stretching vibrations. Raman bands at 553, 571 and 586 cm are assigned to the m4 out of 3À À1 Hydroxyl plane bending modes of the PO4 unit. Raman bands at 432, 457, 479 and 500 cm are attributed to À1 Raman spectroscopy the m2 PO4 and H2PO4 bending modes. In the 2600 to 3800 cm spectral range, Raman bands for whiteite Infrared are found 3426, 3496 and 3552 cmÀ1 are assigned to AlOH stretching vibrations. Broad infrared bands are also found at 3186 cmÀ1. Raman bands at 2939 and 3220 cmÀ1 are assigned to water stretching vibra- tions. Raman spectroscopy complimented with infrared spectroscopy has enabled aspects of the structure of whiteite to be ascertained and compared with that of other phosphate minerals. Ó 2014 Elsevier B.V. All rights reserved. Introduction structural positions, designated X, M(1), and M(2), in that order; for instance, magnesium Mg is always the dominant atom in the The mineral whiteite [1] is a phosphate mineral belonging to M(2) position for all the whiteite minerals [3]. For whiteite, the the jahnsite mineral group [2]. In the whiteite formulae, the Al > Fe in the M3 position; if Fe > Al, then the mineral is jahnsite. symbols in brackets indicate the dominant atom in three distinct Moore and Ito (1978) [4] proposed that the whiteite group, which has the general formula XM(l)M(2)rM(3);+-Jahnsite-(CaMnMn)- ⇑ Corresponding author. Tel.: +61 7 3138 2407; fax: +61 7 3138 1804. (PO4)4(OH)r’HrO, is considered to consist of two series, with the E-mail address: [email protected] (R.L. Frost). M(3) site dominantly Al3+ for the whiteite series and Fe3+ for 1386-1425/$ - see front matter Ó 2014 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.saa.2014.01.053 244 R.L. Frost et al. / Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 124 (2014) 243–248 the jahnsite series. The interesting chemistry of both whiteite and collected at a nominal resolution of 2 cmÀ1 and a precision of jahnsite is these minerals contain multiple cations [5]. ±1 cmÀ1 in the range between 200 and 4000 cmÀ1. Repeated acqui- These two minerals form a continuous series of solid solutions sitions on the crystals using the highest magnification (50Â) were [5]. Whiteite was named after John Sampson White Jr. (born accumulated to improve the signal to noise ratio of the spectra. 1933), associate curator of minerals at the Smithsonian Institute Spectra were calibrated using the 520.5 cmÀ1 line of a silicon wa- and founder, editor and publisher (1970–1982) of the Mineralogi- fer. Previous studies by the authors provide more details of the cal Record. For example: whiteite-(CaFeMg), IMA1975-001, CaFe2+ experimental technique. Alignment of all crystals in a similar ori- 2+ Mg2Al2(PO4)4(OH)2Á8H2O; Whiteite-(MnFeMg), IMA1978-A, Mn entation has been attempted and achieved. However, differences 2+ Fe Mg2Al2(PO4)4(OH)2Á8H2O; Whiteite-(CaMnMg), IMA1986-012, in intensity may be observed due to minor differences in the 2+ 2+ 2+ 2+ CaMn Mg2Al2(PO4)4(OH)2Á8H2O; Rittmannite, Mn Mn Fe 2 crystal orientation. Al2(PO4)4(OH)2Á8H2O [4]. All members of the series belong to the monoclinic crystal sys- Infrared spectroscopy tem with point group 2/m. Most sources give the space group as P2 /a for the Ca Fe rich member, which was the first of the series 1 Infrared spectra were obtained using a Nicolet Nexus 870 FTIR to be described, but Dana gives it as P2/a. The other members spectrometer with a smart endurance single bounce diamond are variously described in different sources as having space groups ATR cell. Spectra over the 4000–525 cmÀ1 range were obtained P2 /a, P2/a or Pa. Whiteite minerals occur as aggregates of tabular 1 by the co-addition of 128 scans with a resolution of 4 cmÀ1 and a crystals, or thick tabular canoe-shaped crystals [3]. Whiteite from mirror velocity of 0.6329 cm/s. Spectra were co-added to improve Rapid Creek in the Yukon Canada [1,2,6,7], is often associated with the signal to noise ratio. deep blue lazulite crystals. Whiteite is invariably twinned, giving Spectral manipulation such as baseline correction/adjustment the crystals a pseudo-orthorhombic appearance and the cleavage and smoothing were performed using the Spectracalc software is good to perfect. The mineral is also located Iron Monarch mine, package GRAMS (Galactic Industries Corporation, NH, USA). Band Iron Knob, Middleback Range, Eyre Peninsula , South Australia and component analysis was undertaken using the Jandel ‘Peakfit’ soft- from the Glen Wills mining district, Omeo, East Gippsland, Victoria, ware package that enabled the type of fitting function to be se- Australia. lected and allows specific parameters to be fixed or varied Raman spectroscopy has proven very useful for the study of accordingly. Band fitting was done using a Lorentzian–Gaussian minerals [8–14]. Indeed, Raman spectroscopy has proven most cross-product function with the minimum number of component useful for the study of diagenetically related minerals where iso- bands used for the fitting process. The Gaussian–Lorentzian ratio morphic substitution may occur as with wardite, cyrilovite and was maintained at values greater than 0.7 and fitting was under- whiteite, as often occurs with minerals containing phosphate taken until reproducible results were obtained with squared corre- groups. This paper is a part of systematic studies of vibrational lations of r2 greater than 0.995. spectra of minerals of secondary origin. The objective of this research is to report the Raman and infrared spectra of whiteite and to relate the spectra to the molecular structure of the mineral. Results and discussion Vibrational spectroscopy background Experimental In aqueous systems, the Raman spectra of phosphate oxyanions Samples description and preparation À1 show a symmetric stretching mode (m1) at 938 cm , an antisym- À1 metric stretching mode (m3) at 1017 cm , a symmetric bending The type locality for whiteite-(CaFeMg) and whiteite-(MnFeMg) À1 À1 mode (m2) at 420 cm and a m4 bending mode at 567 cm is the Ilha claim, Taquaral, Itinga, Jequitinhonha valley, Minas Ger- [16–18]. S.D. Ross in Farmer [19] listed some well-known minerals ais, Brazil, and for whiteite-(CaMnMg) it is the Tip Top Mine (Tip containing phosphate which were either hydrated or hydroxylated Top pegmatite), Fourmile, Custer District, Custer County, Yukon, or both [19]. However not all phosphate minerals were listed and USA [6]. there is a lack of information on anhydrous minerals. The vibra- For the Brazilian whiteite, it is found in association with eosph- tional spectrum of the dihydrogen phosphate anion has been re- orite, zanazziite, wardite, albite, quartz. ported by Farmer [19]. The PO2 symmetric stretching mode The sample was incorporated to the collection of the Geology occurs at 1072 cmÀ1 and the POH symmetric stretching mode at Department of the Federal University of Ouro Preto, Minas Gerais, 878 cmÀ1. The POH antisymmetric stretching mode was found Brazil, with sample code SAC-018. The sample was gently crushed À1 À1 at 947 cm and the P(OH)2 bending mode at 380 cm . The band and the associated minerals were removed under a stereomicro- À1 at 1150 cm was assigned to the PO2 antisymmetric stretching scope Leica MZ4. The whiteite sample was phase analyzed by mode. The position of these bands will shift according to the crystal X-ray diffraction. Scanning electron microscopy (SEM) in the EDS structure of the mineral. mode was applied to support the mineral characterization. The vibrational spectra of phosphate minerals have been pub- Wardite originated from Lavra Da Ilha, Minas Gerais, Brazil.
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