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Experimental Investigation of the Simultaneous Partitioning

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Experimental Investigation of the Simultaneous Partitioning Journal of Mineralogical and Petrological Sciences, J–STAGE Advance Publication, July 22, 2020 Experimental investigation of the simultaneous partitioning of divalent cations between löllingite or safflorite and 2 mol/L aqueous chloride solutions under supercritical conditions Etsuo UCHIDA, Yoshiki SUGINO and Hiroyuki YOKOYAMA Department of Resources and Environmental Engineering, Waseda University, Tokyo 169–8555, Japan In order to elucidate partition behavior of divalent cations between minerals and aqueous chloride solutions under supercritical conditions of fluid phase, we conducted experiments of the simultaneous partitioning of Ni2+,Mg2+, 2+ 2+ 2+ 2+ Co ,Zn ,Fe , and Mn between löllingite (FeAs2)orsafflorite (CoAs2) and 2 mol/L aqueous chloride solu- tions under the conditions of 500 and 600 °C, 100 MPa. Natural löllingite and safflorite were used as starting materials. The bulk partition coefficient (KPB) for the cation partition reactions can be expressed as follows: x – m where MeAs2 indicates the molar fraction of each end member in the solid phase. Meaq is the total molar concentration of Me–bearing aqueous species in aqueous chloride solution. For the experiments using löllingite, the order of partition coefficients of divalent cations was: Co2+ >Fe2+ >Ni2+ >> Mg2+ =Zn2+ ≥ Mn2+, ranging from −4 to 2.3 in logarithm. The order of partition coefficients for safflorite was: Co2+ >Ni2+ >> Fe2+ >Mg2+ >Zn2+ ≥ Mn2+, ranging from −6 to 0.6 in logarithm. The partition coefficient–ionic radius (PC–IR) curves of löllingite and safflorite showed almost no difference between 500 and 600 °C. The PC–IR curves of löllingite and safflorite have a steeper slope than multiple oxide minerals. Mg2+,Co2+,Fe2+, and Mn2+ exhibit partition behavior according to ionic radius. On the other hand, Ni2+ shows a positive partition anomaly in both löllingite and safflorite, whereas Zn2+ shows a large negative partition anomaly that increases with increasing As concentra- tion in the order of pyrite < arsenopyrite < löllingite. Minerals with high ionic bond properties (e.g., ilmenite, magnetite) that have the same 6–fold coordinated sites have a wider PC–IR curve than sulfide, arsenic sulfide, and arsenide minerals with high covalent bond properties. This observation suggests that the selectivity of cations is strong in sulfide, arsenic sulfide, and arsenide minerals with covalent bonds compared with that of multiple oxide minerals with ionic bonds. However, because the electronegativity of arsenic is slightly smaller than that of sulfur, the width of the PC–IR curve seems to slightly narrow in the order of sulfide minerals (pyrite) > arsenic sulfide minerals (arsenopyrite) > arsenide minerals (löllingite). Keywords: Löllingite, Safflorite, Aqueous chloride solution, Partition coefficient, Supercritical condition INTRODUCTION lent cations between various silicate, multiple oxide, and sulfide minerals (e.g., Uchida et al., 2004a, 2004b; Uchi- We have conducted experiments under supercritical con- da and Maruo, 2007; Uchida et al., 2019) and aqueous ditions of the fluid phase under 500–800 °C, 100 MPa to chloride solutions. Similar researches have not been per- determine the simultaneous partitioning behavior of diva- formed by other researchers. In this study, we conducted simultaneous divalent metal cation partition experiments ffl doi:10.2465/jmps.200114Advance Publicationusing löllingite (FeAs2) andArticle sa orite (CoAs2), which are E. Uchida, [email protected] Corresponding author arsenide minerals that have never been tested. Previous 2 E. Uchida, Y. Sugino and H. Yokoyama partition experiments have been reported involving sul- fide minerals, pyrite (FeS2) and pyrrhotite (Fe1−xS) (Uchi- da et al., 2017), which frequently occur in hydrothermal deposits in addition to arsenic sulfide minerals, arsenopy- rite (FeAsS) and cobaltite (CoAsS) (Uchida et al., 2019). The partition coefficient versus ionic radius (PC–IR) curves (Matsui et al., 1977) for pyrite, pyrrhotite, arse- nopyrite, and cobaltite show the similar tendency. In par- Figure 1. Solid starting materials. (a) Löllingite from the Kobushi ticular, Ni2+ shows a positive partition anomaly and Zn2+ mine, Nagano Prefecture, Japan. (b) Safflorite from Timiskam- shows a negative partition anomaly, which is the same as ing District, Ontario, Canada. that reported for multiple oxide minerals such as ilmenite (Uchida et al., 2000) and magnetite (Uchida et al., (Fig. 1b). Because the safflorite ore contains substantial 2004b). However, the widths of the PC–IR curves drawn amounts of calcite, it was crushed to a particle size of from the partitioning of Mg2+,Co2+,Fe2+, and Mn2+ dif- 0.5–1.0 mm and treated with 0.1 mol/L hydrochloric acid fer substantially. The widths for sulfide and arsenic sul- for 2 h to decompose the calcite. Safflorite obtained by fide minerals are much narrower than those of multiple the above treatment was used as starting material. Chemi- oxide minerals, which indicates that minerals in these cal analysis using an energy dispersive X–ray microana- groups have strong selectivity for divalent metal cations. lyzer show that safflorite contained 25.56 ± 0.08 mol% Co, 2.93 ± 0.04 mol% Fe, 2.18 ± 0.06 mol% Ni, 0.46 ± MATERIALS AND METHODS 0.11 mol% Mg, 0.48 ± 0.07 mol% Zn, 0.17 ± 0.03 mol% Mn, 2.67 ± 0.06 mol% S, and 65.55 ± 0.15 mol% As. Solid starting materials Some peaks of cobaltite, kaolinite, and unidentified min- erals were confirmed from powder X–ray diffraction anal- In this study, divalent cation exchange experiments were ysis (Fig. 2c). Löllingite and safflorite form a complete conducted using löllingite (FeAs2)orsafflorite (CoAs2) solid solution in nature (Radcliffe and Berry, 1968). and (Ni, Mg, Co, Zn, Fe, Mn)Cl2 aqueous solutions. Löl- lingite has an ideal chemical composition of FeAs2, be- Liquid starting materials longs to the orthorhombic crystal system, and is classified as a pyrite group mineral (Gaines et al., 1997). Fe occu- A mixture of 2 mol/L aqueous chloride solutions was used pies 6–fold coordinated sites surrounded by six As atoms. as the liquid starting material for reaction with the solid In natural löllingite, Co tends to replace Fe, and S also starting materials (löllingite and safflorite). The chemicals exchanges for As (Gaines et al., 1997). According to Scott used are as follows: reagent grade of NiCl2·6H2O, MgCl2· (1983), löllingite is stable up to temperatures of ~ 700 °C. 6H2O, CoCl2·6H2O, ZnCl2, FeCl2·4H2O, and MnCl2· In this study, we use löllingite from the Kobushi mine, 4H2O (Junsei Chemical Co. Ltd.). In the löllingite experi- Nagano Prefecture, Japan (Fig. 1a) as starting material. ments, an aqueous chloride solution was used by prepar- The löllingite sample was crushed to a particle size of 0.5– ing a mixture of 1 mol/L ZnCl2, CoCl2, NiCl2, MnCl2, and 1.0 mm, and then impurities were removed using tweezers MgCl2 solutions at a volume ratio of 5:2:1:20:20. In the under a stereomicroscope. Chemical analysis using an en- safflorite experiments, an aqueous chloride solution was ergy dispersive X–ray microanalyzer reveals that löllingite used by preparing a mixture of 1 mol/L ZnCl2, FeCl2, contain 30.01 ± 0.15 mol% Fe, 0.75 ± 0.09 mol% Co, 0.06 NiCl2, MnCl2, and MgCl2 solutions at a volume ratio of ± 0.07 mol% Ni, 0.15 ± 0.21 mol% Mg, 0.02 ± 0.06 mol% 5:1:1:20:20. Mn and Mg concentrations were increased in Mn, 0.00 ± 0.07 mol% Zn, 2.34 ± 0.06 mol% S, and 66.67 the starting aqueous chloride solutions in both experiment ± 0.15 mol% As. Minerals other than löllingite were not sets to exceed the lower quantification limit of these ele- detected from powder X–ray diffraction analysis (Fig. 2a). ments in löllingite and safflorite after experiments. The ideal chemical formula for safflorite is CoAs2. Safflorite belongs to the orthorhombic crystal system the Experimental procedure same as löllingite, but is classified as member of the mar- casite group (Gaines et al., 1997). Co occupies 6–fold We combined 30 mg of solid starting material (löllingite coordinated sites surrounded by six As atoms. In natural or safflorite) that had been well ground using an agate safflorite, a significant amount of Fe replaces Co (Gaines mortar, 30 µl of the reaction solution described above, ffl et al., 1997).Advance In this study, sa orite from TimiskamingPublicationand less than 1 mg of anthracene Article (C14H10), which is a re- District, Ontario, Canada was used as starting material ducing agent to keep Fe and Mn in a divalent state in a Cation partitioning between arsenides and aqueous chloride solutions 3 Figure 2. Powder X–ray diffraction patterns of solid starting materials and solid run products. (a) Starting materials of löllingite, (b) solid run products (run no. Lo601) at 600 °C and 100 MPa using löllingite. (c) Starting materials of safflorite. (d) Solid run products (run no. Sa601) at 600 °C and 100 MPa using safflorite. 2+ 2+ 2+ 2+ 2+ 2+ Table 1. Experimental conditions in the FeAs2–(Ni ,Mg ,Co , Table 2. Experimental conditions in the CoAs2–(Ni ,Mg ,Zn , 2+ 2+ 2+ 2+ Zn ,Mn )Cl2–H2O system Fe ,Mn )Cl2–H2O system * ZnCl2:NiCl2:CoCl2:MnCl2:MgCl2 = 5:1:2:20:20 (1 mol/L in total) gold pipe with an outer diameter of 3.0 mm, inner diame- * NiCl2:FeCl2:ZnCl2:MnCl2:MgCl2 = 1:1:5:20:20 (1 mol/L in total) ter of 2.7 mm, and a length of ~ 35 mm that was electri- cally welded on one side. The opposite side of the gold pipe was then sealed by electric welding (Tables 1 and 2) determined target temperature in a horizontal electric fur- and stored in an oven at 105 °C overnight. The weight was nace. The temperature was measured using a chromel– then measured to check whether sealing was complete alumel thermocouple attached to the outer wall of the re- without leakage.
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