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Sphalerite and Aqueous Chloride Solution* MINING GEOLOGY, 42(5), 301•`309, 1992 An Experimental Study on Partitioning of Zn, Fe, Mn and Cd between Sphalerite and Aqueous Chloride Solution* Tomohiro KUBO**, Takayuki NAKATO** and Etsuo UCHIDA** Abstract: The distribution coefficients of Zn, Fe, Mn and Cd between sphalerite and aqueous chloride solution were experi- mentally determined at T=400 and 600•Ž and P=lkbar under relatively reducing conditions. The experiments were con- ducted for the following three systems: ZnS-FeS-(Zn,Fe)Cl2-H2O, ZnS-MnS-(Zn,Mn)Cl2-H2O and ZnS-CdS-(Zn,Cd)Cl2 - H2O systems. The maximum contents of FeS, MnS and CdS in sphalerite were 49, 19 and 24mo1% at 400•Ž and 52, 10 and 15mol% at 600•Ž, respectively. The elements are preferentially partitioned into sphalerite in the order of Cd>Zn>Fe>Mn. This indicates that more covalent elements are preferentially incorporated into sphalerite. The partitioning of the elements becomes more marked with decreasing temperature. gain a better understanding of relative concentra- 1. Introduction tions of these elements in ore-forming solutions. How metallic elements are partitioned between Here we select Fe, Mn and Cd as exchange ele- minerals and coexisting aqueous solution, is an ments, and carry out experiments on the partition- important subject in considering water-mineral ing of these elements between sphalerite and interactions under hydrothermal conditions. In aqueous chloride solution under supercritical con- order to gain such a basic information, we have ditions. The experiments were conducted for the already performed ion exchange experiments be- following three systems: tween minerals and aqueous chloride solution us- (1) ZnS-FeS-(Zn,Fe)Cl2-H2O ing silicates (UCHIDA,1982; KAKUDAet al., 1991; (2) ZnS-MnS-(Zn,Mn)Cl2-H2O OGINOet al., 1992), oxides (KUBOet al., 1992) and (3) ZnS-CdS-(Zn,Cd)Cl2-H2O. and tungstates (UCHIDAet al., 1989). In this study, the ion exchange technique was applied to sphal- 2. Experimental Procedures erite, which is one of the most important sulfide As starting materials for solid phases, ZnS, FeS, minerals and occurs in various types of ore depos- MnS and CdS reagents were used. Each material its. Generally sphalerite contains significant mi- has a purity of >99.99%. As aqueous chloride so- nor elements, such as Fe, Mn, Cd, In and Ga in lutions, 1molal ZnCl2, FeCl2, MnCl2 and CdCl2 varing amounts. The information on the distribu- solutions were prepared prior to the experiments. tion of these elements between sphalerite and The mixture of the solid starting materials (5 to aqueous chloride solution is, therefore, useful to 45mg) and the aqueous chloride solution (20 to Recieved on April 4, 1992, accepted on July 28, 1992 70ƒÊ1) were sealed in a gold capsule with 3.0mm * A part of this study was presented at the Joint Meeting of the outer diameter, 2.7mm inner diameter and 30 to Society of Mining Geologists of Japan, the Mineralogical 40mm in length. For the iron-containing system, a Society of Japan, and the Japanese Association of Mineralo- small amount of anthracene (less than a few milli- gists, Petrologists and Economic Geologists held in Sendai (September 25, 1991) grams) and in some cases, metallic iron as a reduc- ** Department of Mineral Resources Engineering, School of tant were added to the charge to keep iron ion in a Science and Engineering, Waseda University, Ohkubo 3-4- divalent state. All experiments were performed 1, Shinjuku, Tokyo 169, Japan. using standard cold-seal type pressure vessels, Keywords : Ion exchange, Distribution coefficient, Sphalerite, which were heated at the temperature of 400 or Wurtzite, Greenockite, Alabandite, Aqueous chloride 600•Ž in electrical furnaces. The experimental solution. 301 302 T. KUBO, T. NAKATO and E. UCHIDA MINING GEOLOGY : pressure was kept at 1 kbar. The tempera- Table 1 Experimental data for the ion exchange equilibria in the ture was monitored with chromel-alumel system ZnS-FeS-(Zn, Fe)Cl2-H2O at T=400 and 600•Ž and P=1 kbar. thermocouple attached to the outside of the pressure vessel, and the pressure was measured by a Heise gauge. After 7 to 18days at 400•Ž and 5 to 1 7days at 600•Ž, the pressure vessel was rapidly cooled by plunging it into cold water and the charged gold capsule was removed from the vessel. The quench product was washed away from the gold capsule into a beaker with distilled water. The solid product was separated from the aqueous solution using a membrane filter. The solid product was examined using a polarizing microscope, X-ray diffractome- ter and scanning electron microscope, and the chemical composition on the crystal surface was measured using energy disper- sive type X-ray microanalyzers (Link QX200JI and Tracor Northern TN-5400). Cation concentrations in the aqueous solu- tion were determined using an atomic ab- sorption spectrophotometer (Shimadzu AA-610S). 3. Experimental Results 3. 1 ZnS-FeS-(Zn, Fe) Cl2-H2O system The experimental results in the system ZnS-FeS-(Zn,Fe)Cl2-H2O are summarized in Table 1. Solid phases formed in this sys- tem are sphalerite and hexagonal pyrrho- tite. Sphalerite shows a tetrahedral form (Fig. 1-A), and its grain size reaches up to 200ƒÊm in diameter. The maximum FeS content in sphalerite is 49mol% at 400•Ž and 52mo1% at 600•Ž. Hexagonal pyrrho- tite exhibits hexagonal plates (Fig.1-B), and its diameter reaches up to 200ƒÊm. The ZnS content in hexagonal pyrrhotite is neg- ligible. The iron content in pyrrhotite (Table 1) was determined by means of X- ray powder diffractometry using the cali- bration curve relating Fe content to d(102)- spacing by ARNOLD(1962) and TOULMIN and BARTON(1964), assuming that a small amount of Zn has no influence on the d- 42(5). 1992 Partitioning of Zn, Fe, Mn and Cd hetween sphalerite and chioride solution 303 Fig. I Secondary electron images of synthesized minerals. A: sphalerite (XFes=0.056) in the system ZnS-FeS (Run no. K 136, 600•Ž), B: hexagonal pyrrhotite (center) in the system ZnS-FcS, (Run no. K078, 600•Ž), C: manganoan wurtzite (large grains, XMns=0.436) in the system ZnS-MnS (Run no. K118, 600•Ž), D: alabandite(XWS=0.995) in the system ZnS-MnS (Run no. K 121 .600•Ž), E: sphalerite(XCds=0.097) in the system ZnS-CdS (Run no. N 149, 600•Ž), F: greenockite(XCds=0.874) in the system ZnS-CdS (Run no. N 158, 600•Ž). 304 T. Kuao, T. NAKATO and E. UCHIDA MINING GEOLOGY : Table 2 Experimental data for the ion exchange equilibria in the system ZnS-MnS-(Zn, Mn) C12-H20 at T=400 and 600•Ž and P=1 kbar. Fe/(Zn+Fe) mole ratio in solid Fig, 2 Ion exchange isotherms between miner als and aqueous chloride solution in the sys- tem ZnS-FeS-(Zn, Fe)C12 H2O at lkbar. A : 400•Ž and B : 600•Ž. 3.2 ZnS-MnS-(Zn, Mn)Cl2-H2O system The experimental results in the system ZnS- spacing of pyrrhotite. The obtained Fe content in MnS-(Zn, Mn)Cl2-H2O are shown in Table 2. pyrrhotite increases with increasing FeS content Sphalerite, manganoan wurtzite and alabandite in coexisting sphalerite. appeared as solid products. The ion exchange isotherm is presented in the The maximum MnS content in sphalerite de- Roozeboom diagram of Fig.2. The isotherm indi- creases with increasing temperature from 19mol% cates that zinc ion is preferably incorporated into at 400•Ž to 10mol% at 600•Ž due to the prefer- sphalerite, whereas ferrous ion concentrates into ence of wurzite structure at higher temperatures. the aqueous chloride solution. The ion exchange Manganoan wurtzite shows a hexagonal prism isotherms show the temperature dependence, and (Fig. 1-C), and reaches up to 500ƒÊm in length. Its zinc ion is more preferentially partitioned into color is yellowish brown under transmitted light. sphalerite with the decrease of temperature. The The MnS content in manganoan wurtzite ranges Fe / (Zn + Fe) mole ratio in the aqueous chloride from 21 to 26mol% at 400•Ž and from 13 to solution in equilibrium with sphalerite, hexagonal 44mol% at 600•Ž. Its stability field extends with the increase of temperature. The miscibility gap pyrrhotite and metallic iron is 0.97 at 400•Ž and 0.90 at 600•Ž. between sphalerite and manganoan wurtzite is 42(5), 1992 Partitioning of Zn, Fe, Mn and Cd between sphalerite and chioride solution 305 Fig. 3 Ion exchange isotherms between minerals and aqueous chloride solution in the system ZnS-MnS-(Zn, Mn)Cl2-H2O at lkbar. A : 400•Ž and B :600•Ž. Table 3 Experimental data for the ion exchange equilibria in the system ZnS-CdS-(Zn, Cd)Cl2 H2O at T=400 and 600C P=lkbar. very limited. Alabandite shows an octahedral form (Fig.1-D), and is dark green in color under the polarizing microscope. Its grain size is rela- tively small(less than 20ƒÊm). Alabandite contains little ZnS component. The ion exchange isotherm for manganese ion (Fig. 3) shows a remarkable partitioning into the aqueous chloride solution, and this tendency is 306 T. Kuuo, T. NAKATO and E. UCHIDA MINING GEOLOGY enhanced with decreasing temperature. 3.3 ZnS-CdS-(Zn, Cd)Cl2-H2O system The experimental results in the system ZnS- CdS-(Zn, Cd)Cl2-H2O are summarized in Table 3. The minerals appearing in this system are sphaler- ite and greenockite. Sphalerite in this system is fine-grained (less than 10ƒÊm) as compared to that in the previous two systems (Fig. 1-E). The maximum CdS con- tent in sphalerite is 24mol% at 400•Ž and 15mol% at 600•Ž. The stability field of sphalerite dimin- ishes with increasing temperature.
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