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Revision 1 1 2 Synthetic and Natural Ammonium-Bearing Tourmaline 1 Revision 1 2 3 Synthetic and natural ammonium-bearing tourmaline 4 5 Bernd Wunder*1, Eleanor Berryman1,2, Birgit Plessen1, Dieter Rhede1, Monika Koch-Müller1, 6 Wilhelm Heinrich1 7 8 1GeoForschungsZentrum Potsdam, 14473 Potsdam, Germany 9 10 2Fachgebiet Mineralogie-Petrologie, Technische Universität Berlin, 13355 Berlin, Germany 11 12 *E-mail: [email protected] 13 14 ABSTRACT + + 15 Due to the similar ionic radius of K and NH4 , K-silicates can incorporate a 16 significant amount of NH4. As tourmaline is able to accommodate K in its crystal structure at 17 high and ultrahigh pressure, we test if this also holds true for NH4. 18 Piston-cylinder experiments in the system (NH4)2O-MgO-SiO2-Al2O3-B2O3-H2O at 19 4.0 GPa, 700 °C, with B2O3 and NH4OH in excess produce an assemblage of tourmaline, 20 phengite, and coesite. The tourmaline crystals are up to 10 x 40 µm in size. EMP analyses 21 indicate that the tourmalines contain 0.22 (±0.03) wt% (NH4)2O and are solid solutions 22 mainly along the magnesio-foitite and “NH4-dravite” join with the average structural formula X Y Z T 23 ((NH4)0.08(1)☐0.92(1)) (Mg2.28(8)Al0.72(8)) (Al5.93(6)Si0.07(6)) (Si6.00(5)O18)(BO3)3(OH)4 . 24 NH4 incorporation is confirmed by characteristic <N-H> stretching and bending modes in the 25 IR-spectra of single crystals on synthetic tourmaline. Further evidence is the increased unit 26 cell parameters of the tourmaline (a = 15.9214(9) Å, c = 7.1423(5) Å, V = 1567.9(2) Å3) 27 relative to pure magnesio-foitite. 28 Incorporation of NH4 in natural tourmaline was tested in a tourmaline-bearing mica 29 schists from a high P/ low T (> 1.2 GPa/ 550 °C) meta-sedimentary unit of the Erzgebirge, 30 Germany, rich in NH4. The NH4-concentrations in the three main NH4-bearing phases are: 31 biotite (~1400 ppm) > phengite (~700 ppm) > tourmaline (~500 ppm). This indicates that 32 tourmaline can act as important carrier of nitrogen between the crust and the deep Earth 33 which has important implications for a better understanding of the large-scale light element 34 cycle. 35 36 Keywords: Tourmaline, high-pressure synthesis, ammonium, Erzgebirge mica-schists, 37 nitrogen cycle 38 39 INTRODUCTION 40 The transfer of nitrogen from the Earth’s surface to its interior occurs by subduction of 41 ammonium-bearing sediments and altered oceanic crust (e.g., Boyd 2001; Hastings et al. 42 2013; Bebout et al. 2013a; Busigny and Bebout 2013, and references therein). Nitrogen + 43 released from organic matter is predominantly incorporated as NH4 into clay minerals during 44 diagenesis and may subsequently substitute for K+ in K-feldspar, muscovite, biotite and other 45 K-bearing silicates with increasing metamorphic grade (e.g., Williams et al. 1992). There is 46 general agreement that during Barrovian-type metamorphism and during subduction a large 47 proportion of the ammonium is continuously discharged by continuous dehydration reactions 48 (Bebout and Fogel 1992; Bebout et al. 1999; Sadofsky and Bebout 2000; Mingram and 49 Bräuer 2001; Pöter et al. 2004; Pitcairn et al. 2005) and recycled to the surface, for example 50 via arc volcanism. By contrast, high and ultrahigh-pressure, low-temperature metasediments 51 sometimes retain major amounts of NH4 mainly in micas to at least 3.0 GPa and probably 52 beyond (Busigny et al. 2003a; Bebout et al. 2013b). In addition, experiments by Watenphul et 53 al. (2009) have shown that the NH4 analogues of the high-pressure potassium-bearing silicates 54 phengite, K-cymrite, K-hollandite, and K-Si-wadeite are stable to even much higher pressures 55 at relevant temperatures. This indicates that significant amounts of nitrogen can indeed be 56 transported into the deeper mantle. These results are in line with arguments presented by 57 Cartigny and Marty (2013), suggesting that recycling of nitrogen into the mantle presently 58 exceeds outgassing. There is, however, insufficent information about other NH4-bearing 59 minerals that may contribute to the deep nitrogen cycle, as all K-bearing silicates are potential 60 carriers of nitrogen to depth. 61 Tourmaline has been long known as carrier of light elements such as boron and 62 lithium in the Earth’s crust (e.g., Henry and Dutrow 1996; Busigny and Bebout 2013). It 63 forms in various geochemical environments that have undergone diagenetic, metamorphic, 64 metasomatic, or magmatic processes over a wide range of bulk compositions (van Hinsberg et 65 al. 2011), and has a large pressure and temperature stability field ranging from near-surface 66 (Henry et al. 1999) to mantle conditions (Krosse 1995; Marschall et al. 2009). Tourmaline has 67 a very flexible structure, which is able to adjust its composition in response to a wide range of 68 chemical, pressure and temperature variations (Dutrow and Henry 2011) as reflected by its 69 complex general chemical formula, XY3Z6[T6O18](BO3)3V3W (Hawthorne and Henry 1999). 70 The large X site is nine-fold coordinated and typically contains Na, Ca and vacancies (☐) in 71 varying amounts (Hawthorne and Dirlam 2011). K-rich tourmalines are rare (Marschall et al. 72 2009); however, K-dominant tourmalines with up to 0.6 K per formula unit (pfu) have been 73 reported (Grice et al. 1993; Žáček et al. 2000; Shimizu and Ogasawara 2005; 2013). 74 Recent experimental studies at various pressure and temperature (P-T) conditions have 75 shown that in the system MgO-Al2O3-SiO2-B2O3-KCl-(NaCl)-H2O tourmaline may 76 incorporate up to 0.71 K pfu, provided that the pressure is high enough (4.0 GPa, 700 °C) and 77 the bulk composition Na-poor (Berryman et al. 2014; and in prep.). For Na-free bulk 78 compositions, these synthetic tourmalines are mainly solid solutions between the end-member 79 compositions of K-dravite [KMg3Al6Si6O18(BO3)3(OH)3(OH)], Mg-foitite [☐ 80 (Mg2Al)Al6(Si6O18)(BO3)3(OH)3(OH)], and K-olenite [KAl3Al6Si6O18(BO3)3O3(OH)]. Since 81 high pressure encourages the incorporation of K+, this may also hold for the similarly-sized + 82 ammonium ion, NH4 . 83 In this contribution, we test whether high-pressure tourmaline is a potential host for 84 nitrogen by performing experiments in a piston-cylinder apparatus. We will show that 85 magnesio-foitite can accommodate an “NH4-dravite” component up to 8 mole% at 4.0 GPa, 86 700 °C, indicating that tourmaline can transport nitrogen from the Earth’s crust into the 87 mantle. We also measure the nitrogen concentrations in tourmaline coexisting with white 88 mica and biotite from a well-known nitrogen-bearing high-pressure metasedimentary unit of 89 the Erzgebirge (Germany), whose whole-rock nitrogen concentration is ~ 400 ppm (Mingram 90 and Bräuer 2001). Data on NH4-partitioning between micas and tourmaline will demonstrate 91 that tourmaline may constitute a reservoir of nitrogen in metamorphic rocks. We argue that 92 tourmaline is not only important in the transport of boron and lithium but also of nitrogen 93 during large-scale long-term cycling of light elements in subduction processes. 94 95 EXPERIMENTAL AND ANALYTICAL METHODS 96 Experimental procedure 97 NH4-bearing tourmaline was synthesized at 4.0 GPa, 700 °C with a 5-days run 98 duration in a piston-cylinder press. The solid starting material consisted of a homogeneous 99 mixture of SiO2, γ-Al2O3, MgO, and H3BO3 in the stoichiometric proportions of end-member 100 dravite, NaMg3Al6Si6O18(BO3)3(OH)4, without any sodium, and with excess SiO2 and H3BO3. 101 Following the method of tourmaline synthesis from previous studies (von Goerne and Franz 102 2000; Meyer et al. 2008; Berryman et al. 2014) we used excess boric acid in double of the 103 stoichiometric amounts, and excess SiO2 by 20 mole% to compensate for high fluid solubility 104 of these components. About 15 mg of the solid starting material was loaded into a welded 105 gold capsule 10 mm in length and 3 mm in diameter together with ~3 mg of a 25% NH4(OH) 106 solution. The capsule was placed into a high-pressure cell consisting of a steel furnace with 107 fired pyrophyllite and rock salt as pressure media. The pressure uncertainty of this assembly 108 is approximately 1%, calibrated according to the quartz-coesite transition (Mirwald and 109 Massonne 1980). Pressure was maintained within 50 MPa throughout the experiment. The 110 temperature was monitored using a Ni-CrNi thermocouple; its error is estimated to be ±10 °C. 111 At the end of the experiment, the sample was quenched isobarically in less than 15 seconds 112 below 200 °C prior to the slow release of pressure. The capsule was cleaned and reweighed to 113 check for leakage. The smell of ammonia upon opening the capsule indicated that ammonium 114 was available in excess throughout the experiment. The solid product was removed from the 115 capsule and prepared for X-ray powder diffraction, scanning electron microscopy, infrared- 116 analyses and electron microprobe analyses. 117 118 Analytical methods 119 X-ray diffraction (XRD). Powder XRD analysis was performed with a Stoe Stapid P 120 diffractometer operated at 40 kV and 40 mA using CuKα1 radiation collected in the 2θ range 121 5° to 125° with a detector step size of 0.1°, a 2θ resolution of 0.01°, and counting times of up 122 to 20 s per step. Structural parameter and phase proportions were constrained using the GSAS 123 software package for Rietveld refinement (Larson and Von Dreele 2004). The initial structure 124 models were taken from the Inorganic Structure Database (ICSD, FIZ Karlsruhe).
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