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Controls on Tetrahedral Fe(III) Abundance in 2:1 Phyllosilicates

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Controls on Tetrahedral Fe(III) Abundance in 2:1 Phyllosilicates 1 1 (Revision 2) 2 3 Controls on tetrahedral Fe(III) abundance in 2:1 phyllosilicates 4 5 Javier Cuadrosa, Joseph R. Michalskia,b, M. Darby Dyarc, Vesselin Dekovd 6 7 a Department of Earth Sciences, Natural History Museum, Cromwell Road, London SW7 5BD, UK 8 ([email protected]) 9 b Department of Earth Sciences and Laboratory for Space Research, University of Hong Kong, 10 Hong Kong, China ([email protected]) 11 c Department of Astronomy, Mount Holyoke College, South Hadley, MA, 01075 USA 12 ([email protected]) 13 d Department of Ocean Sciences, Tokyo University of Marine Science and Technology, 4-5-7 14 Konan, Minato-ku, Tokyo 108-8477, Japan; e-mail ([email protected]) 15 16 17 18 19 Short title: Controls on tetrahedral Fe(III) in 2:1 phyllosilicates 20 21 Corresponding author: Javier Cuadros; [email protected] 22 23 2 24 ABSTRACT 25 Iron (II) only occupies octahedral sites in phyllosilicates, whereas Fe(III) can occupy both 26 octahedral and tetrahedral sites. The controls on Fe(III) distribution between tetrahedral and 27 octahedral sites have been a matter of great interest in order to understand the interplay between 28 formation environment (Fe abundance, redox conditions) and crystal-chemical factors (stability of 29 the crystal lattice) during crystallization of Fe-phyllosilicates. Here, for the first time, we present a 30 model of Fe(III) distribution in 2:1 phyllosilicates. We investigated 21 samples of 2:1 31 phyllosilicates of submarine hydrothermal origin using XRD, chemical analysis and Mössbauer 32 spectroscopy (and other supporting techniques not presented here). An additional dataset of 49 33 analyses of 2:1 phyllosilicates from the literature was also used. Overall, the data cover a wide 34 range of dioctahedral and trioctahedral phyllosilicates, including endmember minerals and 35 interstratified phases. Dioctahedral phyllosilicates have a steric control whereby tetrahedral Fe(III) 36 is only allowed if at least five out of six octahedral atoms are larger than Al (typically Fe[III], 37 Fe[II], Mg) that produces an expanded structure where tetrahedral sites can accommodate Fe(III). 38 After this threshold, further Fe(III) atoms occupy tetrahedral sites preferentially (~73 % of further 39 Fe[III] atoms) over octahedral sites. In trioctahedral 2:1 phyllosilicates there is no steric hindrance 40 to tetrahedral Fe(III) because the crystal dimensions are such that tetrahedral sites can accommodate 41 Fe(III). On average, Fe(III) enters tetrahedral and octahedral sites in similar proportion, and the 42 only apparent control on tetrahedral Fe(III) abundance is Fe(III) availability during crystallization. 43 This model allows to predict Fe(III) distribution between structural sites, provides an avenue for 44 further exploration of the thermodynamic stability of phyllosilicates using cationic size, and 45 provides a tool to better describe stability/reactivity of Fe-rich phyllosilicates, the most reactive of 46 phyllosilicates and very relevant in geochemical and biological processes. 47 48 Keywords: Dioctahedral 2:1 phyllosilicates; Fe; Tetrahedral Fe; Trioctahedral 2:1 phyllosilicates. 49 3 50 INTRODUCTION 51 Iron-rich phyllosilicates are important because they are more reactive than their Al- and Mg-rich 52 counterparts. Phyllosilicates with significant Fe(II) content, typically trioctahedral, are weathered 53 more rapidly than Al- and Mg-rich ones (Wilson 2004). Iron in phyllosilicates may undergo 54 oxidation and reduction, which has immediate effect on mineral stability, due to modifications to 55 the layer charge. Typically, Fe oxidation state in non-expanding phyllosilicates is not affected by 56 inorganic agents, unless they are extreme (e.g., hydrothermal fluids, strong acid attack). However, 57 microorganisms can modify Fe oxidation state to a certain extent in non-expandable phyllosilicates 58 (e.g., illite, chlorite; Dong et al. 2009). In expandable phyllosilicates (smectite, vermiculite), Fe 59 oxidation state is influenced by both external redox conditions (Fialips et al. 2002) and the direct 60 action of microorganisms (Jaisi et al. 2005). The above reactions are important for microorganism 61 respiration and, more generally, in soils, where water saturation conditions, microbial activity, and 62 organic matter concentration change Fe oxidation state in phyllosilicates. As a consequence, these 63 minerals may experience changes of particle size, particle aggregation state, cation exchange 64 capacity, and even their mineralogy (Stucki et al. 2002; Cuadros 2017). Such changes influence 65 further bio-geochemical processes. Recent articles have demonstrated that Fe in environments with 66 redox fluctuations causes rapid formation of Fe-illite or glauconite from kaolinite or smectite, in 67 reactions of geochemical significance at a global scale (Baldermann et al. 2015; Cuadros et al. 68 2017). As a consequence of all the above, Fe in phyllosilicates promotes faster mineralogical and 69 chemical changes, and a greater, more intense interaction of these minerals with their biological and 70 inorganic environment. Improved understanding of the crystal-chemistry of Fe-phyllosilicates will 71 help to better establish their reactivity. 72 73 Iron most frequently occupies octahedral sites in phyllosilicates. In a first evaluation, it appears that 74 both Fe(II) and Fe(III) fit better within the larger octahedral site than in the smaller tetrahedral site. 75 Iron (III) occupies tetrahedral sites but no Fe(II) has been found so far occupying tetrahedral sites in 4 76 phyllosilicates or, more generally, in silicates. In phyllosilicates, Fe(II) does not enter tetrahedral 77 sites probably due to the combination of large ionic radius (0.71 Å in a tetrahedral environment 78 according to Whittaker and Muntus 1970; compare with the tetrahedral ionic radii of Si and Al of 79 0.26 and 0.39 Å, respectively, from Shannon 1976) and divalent electric charge that does not 80 balance efficiently the negative charge of oxide anions in corner-shared tetrahedra. Iron (III), 81 however, with a trivalent charge and smaller radius (tetrahedral ionic radius of 0.57 Å; Whittaker 82 and Muntus 1970) mitigates totally or partially these hindrances. The distribution of Fe(III) between 83 the tetrahedral and octahedral sheets in phyllosilicates is generally displaced towards the octahedra. 84 It has been frequently assumed that phyllosilicates with low to medium Fe(III) content have no 85 tetrahedral Fe, and thus Fe(III) presence in the tetrahedral sheet is considered only in Fe(III)-rich 86 phyllosilicates. Even in Fe(III)-rich phyllosilicates, if no spectroscopic data were available to 87 establish Fe(III) site location, it was frequently assumed that Fe(III) only enters the tetrahedral sheet 88 if there is not enough Si + Al to occupy it entirely (see Gates et al. 2002, who explained this state of 89 affairs and challenged it). Early studies (1960s and 1970s) reported evidence from Mössbauer 90 spectroscopy that this was not necessarily the case. However, reports of tetrahedral Fe(III) in 91 phyllosilicates have been controversial due to lack of consensus over proper assignment of 92 Mössbauer peaks to structural sites, as discussed below. 93 94 Detection of tetrahedral Fe(III) by Mössbauer faces several obstacles. Because tetrahedral Fe 95 contents are frequently low, the uncertainty associated with the correspondingly low-intensity peaks 96 in the Mössbauer spectra may be high. Further, there is overlap between the low-energy lines (low- 97 velocity values) of tetrahedral Fe(III), octahedral Fe(III) and octahedral Fe(II) (e.g., Coey et al. 98 1984; Rancourt et al. 1992), making it difficult to identify tetrahedral Fe(III) and quantify it. Even if 99 peak positions and relative intensities were correctly identified, their assignment to specific sites is 100 controversial due to the variable range of both isomer shift and quadrupole splitting that Fe(III) 101 displays in tetrahedral and octahedral coordination. Within individual specimens, octahedral Fe(III) 5 102 typically displays two doublets, and possibly three (Drits et al. 1997), generated by different 103 chemical and structural arrangements. Two octahedral Fe(II) peaks are also frequent. Initially, it 104 was suggested that the two octahedral Fe(III) and Fe(II) sites represented cis- and trans-positions 105 (Rozenson and Heller-Kalai 1977), and so were they assigned by several authors. Later studies, 106 however, indicated that cis and trans octahedral sites cannot be resolved either for Fe(III) or Fe(II) 107 (Murad and Wagner 1994; Rancourt 1994; Dyar 2002). As a result of all the above, some peak 108 assignments to tetrahedral Fe(III) have been controversial. For example, the peak assignments to 109 tetrahedral Fe(III) in biotite by Dyar (1990) were contested by Rancourt et al. (1992), and after 110 further discussion and investigation were finally considered most probably caused by Fe(III) in very 111 distorted octahedral sites (Dyar 2002). Similarly, different interpretations of Mössbauer spectra of 112 dioctahedral 2:1 phyllosilicates have led to contrasting tetrahedral Fe(III) contents, more obviously 113 so for low contents (Cardile 1989 and references therein). 114 115 With time, accumulated experience has helped to clarify these issues and provided increasing 116 confidence that Mössbauer spectroscopy can reliably indicate the existence and proportion of 117 Fe(III) in tetrahedral sites (Dyar 2002). There is now evidence that Fe(III) occupies tetrahedral sites 118 even if Si + Al could occupy them entirely. Examples with strong evidence have used combined 119 XANES, EXAFS, near-IR, X-ray diffraction and chemical data on nontronite (Manceau et al. 2000; 120 Gates et al. 2002). Other studies came to the same conclusion using more indirect results, such as 121 infrared investigation of octahedral cations in celadonites and glauconites (Slonimskaya et al. 1986; 122 Besson and Drits 1997; Petit et al. 2015). 123 124 Accordingly, there is no doubt that Fe(III) can occupy tetrahedral sites in phyllosilicates 125 “displacing” Al to the octahedral sheet.
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