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The Crystal Structure of Mineral Fibres. 2 Periodico di Mineralogia (2017) 86, 55-65 PERIODICO di MINERALOGIA An International Journal of established in 1930 Mineralogy, Crystallography, Geochemistry, Ore Deposits, Petrology, Volcanology and applied topics on Environment, Archaeometry and Cultural Heritage The crystal structure of mineral fibres. 2. Amosite and fibrous anthophyllite Simone Pollastri a,*, Natale Perchiazzi b, Lara Gigli c, Paolo Ferretti d, Alessandro Cavallo e, Nicola Bursi Gandolfia , Kilian Pollok f, Alessandro F. Gualtieri a a Department of Chemical and Geological Sciences, University of Modena and Reggio Emilia, Via Campi 103, I-41125 Modena, Italy b Earth Sciences Department, University of Pisa, Via S. Maria 53, I-56126, Pisa, Italy c Elettra-Sincrotrone Trieste S.C.p.A., Strada Statale 14 - km 163,5 in AREA Science Park, I-34149 Basovizza, Trieste, Italy d Museum of Sciences, Via Calepina 14, I-38122 Trento, Italy e Department of Earth and Environmental Sciences, University Milano-Bicocca, I-20126 Milano, Italy f Institut für Geowissenschaften Mineralogie, Friedrich-Schiller-Universität Jena, Carl-Zeiss Promenade 10, D-07745 Jena, Germany ARTICLE INFO ABSTRACT Submitted: January 2017 This study reports for the first time crystal-structure data for amosite and fibrous Accepted: January 2017 anthophyllite. The chemical composition of the two fibre species was determined Available on line: March 2017 from EMPA. Crystal structures were refined using powder-diffraction data, using both laboratory sources and synchrotron radiation. Results were compared with the available * Corresponding author: literature data for the non-fibrous varieties grunerite and anthophyllite, respectively. [email protected] The calculated site-occupancies for all samples are in agreement with the chemical compositions calculated from EMPA. The existing structure models of grunerite and DOI: 10.2451/2017PM693 orthorhombic anthophyllite also applies to the corresponding fibrous varieties amosite and fibrous anthophyllite, respectively. In amosite, bothFe 2+ and Fe3+ atoms are found at How to cite this article: the sites M(1), M(2) and M(3) and Fe2+ ions is the only atomic species found at site M(4). Pollastri S. et al. (2017) Period. Mineral. 86, 55-65 Mg is disordered over the C sites with a preference for site M(2). Minor Ca and Na have been assigned to the A site. In fibrous anthophyllite, Mg is the only atomic species found at the M1, M2 and M3 sites. Fe2+, Mg (and minor Mn) have been assigned to the M4 site, whereas minor Ca has been assigned to the A site. In both structures, the environment at the M(4) site in amosite and M4 site in fibrous anthophyllite is highly distorted. This work can be considered a basis for studies aimed at understanding the potential toxicity/ pathogenicity of these mineral fibres. Keywords: Mineral fibres; amphibole; Rietveld; crystal-structure refinement; iron. INTRODUCTION and Redlich, 2015; Huang et al., 2011; Mossman et al., Asbestos minerals (fibrous amphiboles and chrysotile; 2011; Roe and Stella, 2015). Despite the large number of IARC, 1973; USGS, 2001) together with fibrous zeolites studies over the last twenty years (see for example: Kamp, such as erionite, are the most common mineral fibres. 2009; Huang et al., 2011; Liu et al., 2013; Mossman et The dreadful reputation of asbestos minerals is due to the al., 2011), the mechanisms by which asbestos, and onset of malignant lung diseases, mainly lung carcinoma mineral fibres in general, induce cyto- and geno-toxic and pleural/peritoneal malignant mesothelioma (MM), damage remain poorly understood. This is due to their following their inhalation (see for reviews: Broaddus great chemical variability and atomic arrangements, in et al., 2011; Bunderson-Schelvan et al., 2011; Gulati addition to other factors (fibre size, surface reactivity, PM 56 Periodico di Mineralogia (2017) 86, 55-65 Pollastri S. et al. biopersistence, iron oxidation state/coordination number) Micro-Probe Analysis (EMPA) and X-Ray powder- that contribute to biogeochemical reactions (Fubini and diffraction (XRPD) experiments using both lab sources Mollo, 1995; Hardy and Aust, 1995; Donaldson et al., and synchrotron radiation. A special attention was paid to 2010). This work is framed within the long-term research the occupancy of iron because it is considered to play a project entitled “Sviluppo di un modello generale di major role in the pathogenicity of the fibres, as it generates interazioni tra fibre minerali e cellule biologiche”, part of reactive oxygen species (ROS), mobilization by chelators the Italian Research Project of National Interest (PRIN), and catalysed reactions (Hardy and Aust, 1995). in progress since 2011, aimed at understanding the nature of biological interaction mechanisms of mineral fibres of MATERIALS AND METHODS socio-economic and industrial importance and to develop Sample selection and preparation a general model of fibre toxicity. The model could be The fibrous amphiboles selected for the study are: useful to assess the potential toxicity and pathogenicity - the UICC standard amosite asbestos (South African, 2+ 2+ of unclassified and unregulated fibres, preventing new NB #4173-111-4) (ideal formula Fe 2Fe 5[Si8O22] cases of mass exposure such as those reported for the (OH)2 and space group C2/m) from Penge mine, Northern fluoro-edenite (Comba et al., 2003) and fibrous erionite Province (South Africa) (Dumortier et al., 2001). To achieve this goal, full - the UICC standard anthophyllite asbestos (Finnish NB mineralogical and crystallographic characterization of the #4173-111-5) (ideal formula Mg2Mg5[Si8O22](OH)2 fibres is of paramount importance and can be used as a and space group Pnma) from Paakkila (Finland). basis to understand the chemical/physical and biological The surface reactivity, chemical environment of iron, properties relevant to toxicity and pathogenicity. thermal behaviour and trace elements in the samples have Amphiboles are double-chain silicates with a Si(Al):O been already investigated by our group and published ratio of 4:11. The oxygen atoms of the chains can elsewhere (Pollastri et al., 2014; 2015; Bloise et al., 2015; coordinate Si(Al) and also a variety of other cations sites; 2016). the simplified general formula for amphiboles, following Samples were manually ground in agate mortar prior to Hawthorne et al. (2012) is: A0-1B2C5T8O22W2. The anions the X-ray diffraction investigation. W (OH, F, Cl, O2-) occur at the O(3) site, T (Si4+, Al3+) are the tetrahedrally coordinated sites within the silicate Experimental and data analysis chain, the C cations (Mg2+, Fe2+, Mn2+, Al3+, Fe3+, Ti3+, EMPA were done using a JEOL 8200 Super Probe Ti4+ Li+, Mn3+) occur at the octahedrally coordinated sites instrument with W hairpin-type filament and minimum M(1), M(2) and M(3) in monoclinic amphiboles, the B accelerating voltage of 30 kV. The content of H2O was cations (Na+, Li+, Ca2+, Mn2+, Fe2+, Mg2+) occur at the independently determined on the very same samples [8]-coordinated M(4) site in monoclinic amphiboles, and with Thermogravimetric (TG) analysis (taken from the A cations (Na+, K+, Ca2+, Li+) occur in the A cavity the literature; Bloise et al., 2015). The final chemical with coordination number from [6] to [12]. compositions are the mean values of several analyses In the frame of the project, the chemical environment carried out on various fibres (not less than 10 per sample). of iron in the crystal structure of these mineral fibres The calculation of the crystal-chemical formula was has been recently investigated (Pollastri et al., 2015) normalized on the basis of 24 O. The assignment of Fe2+ through a combined X-ray absorption and Mössbauer and Fe3+ was possible using independent Mössbauer spectroscopic study. The results confirm that amphibole data (Pollastri et al., 2015). Cations reported in atoms asbestos fibres host iron in octahedrally coordinated sites, per formula unit (a.p.f.u.) were assigned following in perfect agreement with previous studies (Whittaker, the schemes proposed by Hawthorne et al. (2008) for 1949; Bancroft et al., 1966; Whitfield and Freeman, 1967; anthophyllite and by Hawthorne and Oberti (2007) and Cameron and Papike, 1979; Stroink et al., 1980). Leake et al. (1997) for amosite. Our work is along the research line of the crystal High-resolution XRPD pattern of amosite was collected chemical characterization of fibrous amphiboles such as at the MS-X04SA beamline, SLS, Villigen, Switzerland. fluoro-edenite (Gianfagna et al., 2003; Gianfagna et al., The beamline is powered by a short-period (14 mm) 2007; Andreozzi et al., 2009) fibrous tremolite (Ballirano in-vacuum, cryogenically cooled, permanent-magnet et al., 2008; Pacella et al., 2008) fibrous richterite (Pacella undulator (CPMU, U14). The diffractometer has Debye- and Ballirano, 2016) and winchite (Gunter et al., 2003). Scherrer geometry and is equipped with a solid-state This study reports for the first time crystal-structure silicon-microstrip detector, called MYTHEN (Microstrip data for amosite and fibrous anthophyllite, two of the sYstem for Time-rEsolved experimeNts). A detailed fibrous amphiboles classified as asbestos so that all the description of the beamline is reported in Willmott et al. structure models of the five amphibole asbestos species (2013). The sample powder was inserted in a borosilicate are now available. Samples were investigated by Electron capillary 0.3 mm in diameter and data were collected PM Crystal structure of amosite and anthophyllite 57 by spinning the capillary. The wavelength used for the The background profile was fitted with a Chebyshev experiment was 0.775 Å. polynomial function with a variable number of coefficients The XRPD pattern of anthophyllite was collected using depending on the complexity of the background curve. a conventional Bragg–Brentano PANalytical X’Pert Pro The diffraction peak profiles were modelled using a diffractometer, with Θ–Θ geometry, CuKα radiation, pseudo-Voigt function with a q-independent Gaussian 40 kV and 40 mA and an RTMS (Real-Time Multiple- and two Lorentzian coefficients. The unit-cell parameters Strip) detector.
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