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Yamanaka, T., Maeto, K., Akashi, H., Ishibashi, J.-I., Miyoshi, Y., Okamura, K., Noguchi, T., Kuwahara, Y., Toki, T., Tsunogai, U., Ura, T., Nakatani, T., Maki, T., Kubokawa, K. and Chiba, H. (2013) Shallow submarine hydrothermal activity with significant contribution of magmatic water producing talc chimneys in the Wakamiko Crater of Kagoshima Bay, southern Kyushu, Japan. Journal of Volcanology and Geothermal Research. 258, 74-84.
Zheng, L.-W., Hsiao, S. S.-Y., Ding, X.-D., Li, D., Chang, Y.-P. and Kao, S.-J. (2015) Isotopic composition and speciation of sedimentary nitrogen and carbon in the Okinawa Trough over the past 30 ka. Paleoceanography, 30, 1233–1244.
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Supplementary Table 1. Nitrogen contents and nitrogen isotopic values of tobelite before and after treatment.
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Supplementary Table 2. TOC and TN contents and δ N values of TN in the bulk sediments obtained by a piston corer in the Wakamiko Crater.
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Appendix Fig. 1. The proportion of mineral nitrogen (MN) and adsorbed nitrogen (TNAd) contents for total nitrogen of clay fraction (TNC.F) at sampling site. a) 2-26 cmbsf in the 1091MB core, b) 10-22 cmbsf in the 1093MG core, c) 5-19 cmbsf in the 1094MR core, d) 0-19 cmbsf in the 1094MY core, e) 0-24 cmbsf in the 1097MR core, f) 0-7 cmbsf in the 1101MY core.
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Chapter-2: Synthesis of ammonium containing 2:1 clay minerals under the hydrothermal conditions at 200ºC and saturated vapor pressure
1. Introduction
The synthesis of ammonium-bearing clay mineral under hydrothermal conditions have been reported by many researchers (Chourabi and Fripiat, 1981; Gautier et al., 2010; Kloprogge et al., 1993; Kloprogge, 1994; Kloprogge et al., 2006; Kloprogge et al., 1999; Petit et al., 2006; Petit et al., 1999; Petit et al., 1998; Šucha et al., 1998;
Vogels et al., 1997; Zhang et al., 2010). Ammonium has been known to present as an exchangeable cation in interlayers of 2:1 clay mineral (Aranda and Ruiz-Hitzky, 1999; Gautier et al., 2010; Vogels et al., 1997).
Negatively charged 2:1 layers could be neutralized by several ways as follows:
1) replacement of Al3+ for Si4+ in the tetrahedral layers, 2) replacement of Mg2+ for Al3+ in the octahedral layers (Kloprogge and Kaomarneni, 1999; Perry and Hower, 1970). An exchangeable cations, including ammonium, coexist with nH2O molecules in interlayers of 2:1 clay mineral, which play a role of neutralization for imbalanced ionic charge in the layers (Hendricks et al., 1940; Aranda and Ruiz-Hitzky, 1999; Gautier et al., 2010; Hendricks et al., 1940).
In order for cation to fix in the interlayer, the electrostatic attraction between the cation and interlayer surface must exceed the energy of hydration so that water molecules can be excluded from the interlayer space (Hurst and Jordine, 1964;
Kittrick, 1966). In other words, if the electrostatic attraction between negatively charged 2:1 layers and exchangeable cations become stronger than those between cations and the shell of hydrating water molecules, smectite could be converted to a mica-like layer (Perry and Hower, 1970). For example, ammonium cation can coexist as exchangeable and fixed form in interlayers of 2:1 clay mineral (Hall,
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1999; Matsuoka and Moritsuka, 2011; Williams et al., 1989), it can be detected by FT-IR analysis based on the absorptions of N–H-bending and N–H-stretching (Aranda and Ruiz-Hitzky, 1999; Petit et al., 1999; Petit et al., 1998; Pironon et al., 2003; Russell and White, 1966).
Under these background, the main purpose of this study is the synthesis of ammonium containing 2:1 clay mineral from various starting materials under the hydrothermal conditions at 200 ºC and saturated vapor pressure. In addition, it is to observe the incorporation of ammonium in interlayers of 2:1 clay mineral after saturation with high concentrations of ammonium solution. This study will give us an important information about ammonium distribution in 2:1 clay mineral formed under the high concentrations of dissolved ammonium conditions.