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CHEMICAL REACTIONS AMONG CLAY MINERALS' CALCIUM CARBONATE, and AMMONIUM CHLORIDE Snrcnrr Iw.Q.Iuoro Anl Tosnro Suoo, Geologicol

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CHEMICAL REACTIONS AMONG CLAY MINERALS' CALCIUM CARBONATE, and AMMONIUM CHLORIDE Snrcnrr Iw.Q.Iuoro Anl Tosnro Suoo, Geologicol THE AMERICAN MINERALOGIST, VOL. 50, JULY_AUGUST' 1965 CHEMICAL REACTIONS AMONG CLAY MINERALS' CALCIUM CARBONATE, AND AMMONIUM CHLORIDE snrcnrr Iw.q.iuoroaNl Tosnro suoo, Geologicoland, Minerological Institute, Foculty of Science,Tohyo Uni,ttersi'tyof Eilucation, Otsuka, Tokyo, JaPan. Ansrnacr Various kinds of ciay minerals mixed with calcium carbonate and ammonium chloride and the i,vere heated at a specific temperature in the range oi 500-1000" c. Ior one hour, reaction products were examined. The kinds of reaction products depend upon the chemical compositions of the clay minerals. In the case of clay minerals rich in aluminum, formation of such minerals as hydrogrossularite, wollastonite, haiiyne, larnite, etc., was observed. periclase, with clay minerals rich in magnesium, crystallization oI such minerals as both forsterite; monticellite, spurrite, etc., was observed. For clay minerals containing and aluminum and magnesium, such minerals as periclase, forsterite, hydrogrossularite, monticellite ll'ere formed. When calcium carbonate alone was used, the crystallization chloride temperatures usually rose higher than those in the case when both ammonium and calcium carbonate -".e used, the kinds of reaction products differed, particularly in clay minerals rich in aluminuml gehlenite was noticed as one of the principal reaction products. Probably chlorine acts on calcium ions forming calcium chloride, which reacts may with silicates. Hydrogen in ammonium ions released from ammonium chloride play an important role in the formation of hydrogarnet. INrnooucrtoN The authors have taken an interest in chemical reactions among sili- cates or volcanic glass and various kinds of alkali-earth salts or metal oxides under a specific chemical environment in which catalytic reac- tions are suggested(Sudo and Matsuoka, 1959; Ueda and Sudo, 1963)' In relation to this, the authors have investigated the chemical reaction in the processof the Smith method (1871) which has long been used in the chemical analysis for alkalies. In a preliminary report (Sudo, el at.1960), the authors reported the formation of hydrogrossulariteand periclase from leuchtenbergite. In the present work, the experiments were extended by using various kinds of clay minerals as starting ma- terials, and the formation of various kinds of reaction products, which are usually found in nature as skarn minerals, was revealed' The re- sults of these experiments revealed that a volatile material such as ammonium chlorid,eplays an important role in promoting complicated chemical reactions among clay minerals, ammonium chloride and calcium carbonate. In this connection, the authors refer to the work of Gorgeu who, in 1883,reported the possibility of the synthesisof grossulariteby passing hydrogen and steam over a mixture of pipe clay (pyrophyllite) and calcium chloride in a platinum crucible. 886 CLAY MINERAL REAC:TIONS 887 SranrrNc MerBnrars The following clay minerals were used as startinq materials: (a) rllite from Yoji, Gumma Prefecture. rt occurs as a hydrothermal alteration product of granodiorite (Kodama, 1957). (b) Pyrophyllite from Yoji, Gumma Prefecture. rt occurs as a hydrothermal alteration product of shale (Kodama, 1958). (c) Montmorillonite from Endani, Tottori Prefecture. It occurs as clay veins cutting granite (Yoshikawa and Sudo, 1960). (d) Leuchtenbergite from the wanibuchi mine, shimane prefecture. rt occurs in the alteration area around the hydrothermal replacement bodies of glpsum in Tertiary tuffs or volcanic rocks (Sakamoto and Sudo, 1956). (e) Kaolinite from the Kampaku mine, Tochigi Prefecture. It occurs as a hydrothermal alteration product of liparite around gold-quartz vein. (f) Antigorite from llaruyama, Iwate prefecture. (g) Vermiculite from Gobangumi, Fukushima Prefecture. It occurs in sementine near the contact with granite. (h) Talc from Atihata, Gumma Prefecture. (i) Hydrated halloysite from the ZuihO mine, Taiwan and from the Jdshin mine, Gumma Prefecture. The former occurs as a gangue mineral of gold-quartz veins, and the Iatter occurs as a hydrothermal alteration product of andesite (sudo and ossaka, 1952). (j) Allophane from Oya, Tochigi Prefecture. It occurs as a weathering product of pumice fragments in the surface soil (Sudo and Ossaka, 1952). The chemical compositions of these starting materials are shown in Table 1. ExpBnruBNrs The starting materials are free of impurities as far as the detection limit of the usual c-ray diffractometer recording. Each sample was directly pulverized in an agate mortar into fine powder and its size was set below 5 microns by decantation. The sample was mixed with cal- cium carbonate (reagent grade) and ammonium chloride (reagent grade) in various molecular ratios. The weight of the mixture was set at 0.5 g throughout the experiments. Each mixture was heated at every 100o temperature,namel)' 100oC., 200oC., . , 1000oC., for one hour at a mean heating rate of 20o C. per minute. The mixture was kept at a specific temperature for one hour and then cooled immediately. After cooling to room temperature, the content of the crucible was put into boiling water for 15 minutes to one hour; then it was filtered, and washed with distilled water to remove the water-soluble products completely. The residue thus obtained was dried at 100-110o C. and examined by an xc-raydiffractometer. RBacrroN Pnopucrs Experimental data are given in Table 2. Table 3 showsthe rise and fall of the amounts of reaction of cla_vmineral: CaCOa:NHnCl. 888 S. IWAMOTO AND T. SUDO T,\er,B 1. Crrnurcer-CouposrrroNs or. rrrr Srentruc Metnnurs (a) (b) (c) (d) (e) (f) (s) (h) Sioz 47.63% 62.02T0 48.907029 .O7', o 41.77o'o41.++a t 25.060 a 38.977a Tio, 0.10 tr. 0.32 0.05 0.12 AlrOs 37.03 32'24 18.40 21.82 35.70 0.95 27.68 3+.43 FezOa 0.01 tr. 1.r2 0.83 0.40 1.56 t .24 2.06 FeO tr. tr. 0.01 3.67 1.79 MsO 0.04 0.18 1.88 29.90 0.84 4t .06 0.59 CaO tr. 0.04 2.25 0.19 tr. 0.11 1.59 MnO tr. none 0.04 NarO 0.76 0.35 0.35 0.04 0.10 KzO 9.02 0.28 tr. 0.16 none 10.s8 13.90 I^. -. H,O(+) 4.97 \^ n^ 8.44 r0.76 13.25 H,O(-) 0.73 J"'"" 17.64 2.76 4.33 2.12 20.82 lz+'oo PzOr 0.02 0.05 0.02 Total 100.317a100.54ok gg.327a 99.67a/o 99.547a 99.897a (90'88%)1O0'127a (a) Illite, Yoji, Gumma Prefecture (Kodama, 1957). (b) Pyrophyllite, Yoji, Gumma Prefecture (Kodama, 1958). (c) Montmorillonite, Endani, Tottori Prefecture (Yoshikau'a and Sudo, 1960)' (d) Leuchtenbergite, Wanibuchi mine, Shimane Prefecture (Sakamoto and Sudo, 19s6). (e) Kaolinite, Kampaku mine, Tochigi Prefecture (Iwai and Kuroda, 1960)' (f) Antigorite, Haruyama, Iwate Prefecture (Analyst: the authors)' (g) Allophane, Oya, Tochigi Prefecture (Sudo and Ossaka, 1952, analyst: Hideo Minato). 1959, (h) Hydrated halloysite, Joshin mine, Gumma Prefecture (Sudo and Ossaka, analyst: Geological Survey of Japan). Illite: In the range of the following Proportions, illite:CaCOa:NH4CI : 1:0-5: 2-10, the crystallizatiorl of the minerals such as anorthite' hydrogrossularite (CasAlr(Si04)a--(OH)o*),a cancrinite-like mineral with main reflections; 4.77 h (relative intensitl:69), 3.69 A (SO), 3.28A (r00),2.g2e.(io), 2.76 hQ8),2.65 A (51),2.45A (31),2.127 ]\ (40), 1.781A (tO), and an undeterminedmineral was observed.H-vdro- grossuiaritetends to be formed when the ratio of CaCOais relativel.v higher. The chemical compositionof the residue obtained in the ratio of illite:CaCOs:NH4CI:1:4:8, heatedat 900" C., is as shownin Table 4a. Pyrophyltite.'In the caseof sucha ratio as pyrophyllite: CaCOa:NH+CI : 1:5: 10, the crystallization of pseudowollastonite'hydrogrossularite, and hailyne was noticed.l As the temperature rose' haiiyne disappeared, 1 Identification of haiiyne was only based on the principal r-ray powder reflections' Although the general formula of haiilme is given as (Na, Ca)r-sA16Si6O%(SO4,S)r-:, it is CLAV MINERAL REACTIONS 889 pseudowollastoniteand hydrogrossularite remained, and successivelvthe growth of hydrogrossularitewas enhanced. -[he Montmorillonite: starting materia] contains a small amount of quartz, which could hardly be removed by the sedimentation method. The results obtained, using the original sample, are as follows; in the ratio of montmorillonite:CaCOa:NH+CI:1:4:8,the formation of such minerals as hydrogrossularite, pseudowolrastoniteand wollastonite was observed. The reflectionsof pseudowollastoniteand hydrogrossularite gradually increasewith increasingtemperature. V ermiculite: In the ratio of vermiculite: CaCOa:NH4CI : 1: 4 : g, the crystallization of minerais such as hydrogrossularite, monticellite and periclase was obtained. The reflections of monticellite are weak, but thoseof hydrogross.laritewere graduariyenhanced with rising tempera- ture. Leuchtenbergite:In the ratio of leuchtenbergite:CaCOs: NH4CI: 1:4-5: 10, the crystallization of the minerals such as hydrogrossularite,periclase, larnite (CarSiOa)and spurrite (2 Ca2SiOa.CaCOa)was observed.The reflections of periclase and hydrogrossularite were gradually enhanced with rising temperature, and spurrite and larnite were found only at a high temperature in associationwith periclaseand hydrogrossularite. The residue obtained under the conditions of the ratio 1:5:10 and 900' c. was analyzed chemically (Table 4b). The oxide ratio is obtained as 3.1CaO.AlrOs.2.4SiOz. l.9H2O+3.2MgO, which correspondsto the composition of a mixture of hydrogrossularite and periclasein a molec- ular ratio of nearly 1:3. Talc: In the ratio of talc:CaCOs:NH4CI:1:0-6:8, the formation of the minerals such as enstatite, diopside, monticellite, spurrite and merwinite (cagMgSiros)was observed.Enstatite was only formed in the casewithout caco3, henceit is appropriately inferred that enstatite is a firing product of talc itself.2 The formation of monticellite was clearly confirmed in the range of CaCO3:2-6, and 600-1000" C. When a product, which was obtained at 800" c.
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