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Acquisition and Evaluation of Thermodynamic Data for Morenosite-Retgersite Equilibria at 0.1 Mpa

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Acquisition and Evaluation of Thermodynamic Data for Morenosite-Retgersite Equilibria at 0.1 Mpa University of Nebraska - Lincoln DigitalCommons@University of Nebraska - Lincoln USGS Staff -- Published Research US Geological Survey 2003 Acquisition and Evaluation of Thermodynamic Data for Morenosite-Retgersite Equilibria at 0.1 MPa I-Ming Chou 954 National Center, U.S. Geological Survey, Reston, Virginia 20192, U.S.A., [email protected] Robert R. Seal II 954 National Center, U.S. Geological Survey, Reston, Virginia 20192, U.S.A. Follow this and additional works at: https://digitalcommons.unl.edu/usgsstaffpub Part of the Earth Sciences Commons Chou, I-Ming and Seal II, Robert R., "Acquisition and Evaluation of Thermodynamic Data for Morenosite- Retgersite Equilibria at 0.1 MPa" (2003). USGS Staff -- Published Research. 328. https://digitalcommons.unl.edu/usgsstaffpub/328 This Article is brought to you for free and open access by the US Geological Survey at DigitalCommons@University of Nebraska - Lincoln. It has been accepted for inclusion in USGS Staff -- Published Research by an authorized administrator of DigitalCommons@University of Nebraska - Lincoln. American Mineralogist, Volume 88, pages 1943–1948, 2003 Acquisition and evaluation of thermodynamic data for morenosite-retgersite equilibria at 0.1 MPa I-MING CHOU* AND ROBERT R. SEAL II 954 National Center, U.S. Geological Survey, Reston, Virginia 20192, U.S.A. ABSTRACT Metal-sulfate salts in mine drainage environments commonly occur as solid solutions containing Fe, Cu, Mg, Zn, Al, Mn, Ni, Co, Cd, and other elements. Thermodynamic data for some of the end- member salts containing Fe, Cu, Zn, and Mg have been collected and evaluated previously, and the present study extends to the system containing Ni. Morenosite (NiSO4·7H2O)-retgersite (NiSO4·6H2O) equilibria were determined along five humidity buffer curves at 0.1 MPa and between 5 and 22 rC. Reversals along these humidity-buffer curves yield ln K = 17.58–6303.35/T, where K is the equilib- rium constant, and T is temperature in K. The derived standard Gibbs free energy of reaction is 8.84 kJ/mol, which agrees very well with the values of 8.90, 8.83, and 8.85 kJ/mol based on the vapor pressure measurements of Schumb (1923), Bonnell and Burridge (1935), and Stout et al. (1966), respectively. This value also agrees reasonably well with the values of 8.65 and 9.56 kJ/mol calculated from the data compiled by Wagman et al. (1982) and DeKock (1982), respectively. The temperature– humidity relationships defined by this study for dehydration equilibria between morenosite and retgersite explain the more common occurrence of retgersite relative to morenosite in nature. 2+ INTRODUCTION systems, such as the Fe SO4–H2O system, temperature-depen- Efflorescent metal-sulfate salts have been demonstrated to dent equilibria among four or more solids can be described by play an important role in metal cycling in acid mine-drainage simple dehydration reactions. Thus, recent development of the environments (Dagenhart 1980; Jambor et al. 2000). The salts humidity-buffer technique provides an efficient and reliable form through evaporative processes in all climates and pro- method for obtaining and evaluating these data (Chou et al. vide a means of storing acidity and metals. Their rapid and 2002). To establish a useful thermodynamic database for the high solubilities cause acute toxic effects to aquatic ecosys- interpretation of natural assemblages, it is first necessary to tems during spring-melt events in areas with winter snow cover, study thermodynamic properties of end-member sulfate salts and during rainstorm events. (Chou et al. 2000, 2002 for Fe and Cu; Chou and Seal 2001a, Efflorescent sulfate salts of Fe—both Fe2+ and Fe3+—such in preparation, for Zn; and Chou and Seal 2001b, 2003, for 2+ 2+ Mg). The present study extends the database to the Ni sulfate as melanterite [Fe SO4·7H2O], rozenite [Fe SO4·4H2O], and 2+ 3+ system. Dissolved Ni has known toxicity to aquatic ecosys- copiapite [Fe Fe 4(SO4)6(OH)2·20H2O], and salts of Al, such tems in a variety of mine drainage settings. as alunogen [Al2(SO4)3·17H2O] and halotrichite-pickeringite [(Fe2+, Mg)Al (SO ) ·22H O], are common in mine-waste set- 2 4 4 2 Mineralogy of nickel sulfates tings. However, salts dominated by other, less abundant metals such as Cu, Zn, Ni, and others also occur locally (Jambor et al. Morenosite is a member of the epsomite group, which con- 2000). More important from an environmental perspective, toxic sists of orthorhombic (P212121) sulfate heptahydrate minerals 2+ trace metals commonly occur in solid solution in the more com- of the type M SO4·7H2O, where M represents Mg (epsomite), mon hydrated Fe-sulfate salts such as melanterite, rozenite, or Ni (morenosite), and Zn (goslarite). In contrast, the common 2+ the Fe2+ sulfate pentahydrate–siderotil. Melanterite has been Fe sulfate heptahydrate, melanterite [FeSO4·7H2O], is mono- documented experimentally and in nature containing close to 45 clinic. Morenosite apparently forms complete solid solutions mol% Cu, 40 mol% Zn, and 20 mol% Ni (Jambor et al. 2000). with the Mg and Zn end-members (Jambor et al. 2000). In the The ability to model the geochemical behavior of these min- presence of an aqueous solution, morenosite is not stable at erals and their trace elements in aquatic environments relies on temperatures above about 31.2 rC and dehydrates to form the availability of accurate and precise thermodynamic data retgersite (Linke and Seidell 1965). for these phases and their solid solutions. The ability to model Retgersite [a-NiSO4·6H2O] is bluish green and tetragonal solid solutions depends not only on reliable data for the mix- in crystal form. It is stable between 31.2 and 53.3 rC (Linke ing properties of these minerals, but also on the data for end- and Seidell 1965). Above 53.3 rC, the crystals turn green and member compositions of hydrated trace metal sulfates. form nickelhexahydrite [b-NiSO4·6H2O]. Nickelhexahydrite Thermodynamic data for many of these minerals have not been is one of the six members of the hexahydrite group, which available, or were of poor quality until recently. For all of these are monoclinic (C2/c) sulfate minerals of the type 2+ M SO4·6H2O, where M represents Mg (hexahydrite), Mn (chvaleticeite), Fe (ferrohexahydrite), Ni (nickelhexahydrite), * E-mail: [email protected] Co (moorhouseite), and Zn (bianchite). Even though little is 0003-004X/03/1112–1943$05.00 1943 1944 CHOU AND SEAL: MORENOSITE-RETGERSITE EQUILIBRIA known about the limits of solid solution in these hexahydrates, substitution of up to 27 mol% Ni for Mg has been reported for natural hexahydrite (Janjic et al. 1980). Except for hexahydrite, minerals of the group occur sparingly as the oxidation prod- ucts of sulfide deposits (Jambor et al. 2000). Dehydration equilibrium The stability of morenosite and retgersite can be related by the reaction: NiSO4·7H2O(s) = NiSO4·6H2O(s) + H2O(g) (1) morenosite retgersite where (s) and (g) are solid and gas, respectively. Published es- timates for the equilibrium relative humidity (RH) at 25 rC range from 67 to 96% for the reaction. To evaluate these data, FIGURE 1. Morenosite [NiSO ·7H O]-retgersite [NiSO ·6H O] the humidity-buffer technique (Polyanskii et al. 1976; Malinin 4 2 4 2 equilibria at 0.1 MPa. Result of vapor-pressure measurement at 0.1 et al. 1977, 1979; Chou et al. 1998a, 1998b, 1999, Chou et al. MPa and 25 rC by Schumb (1923) is shown by the square. Also shown 2002) was used in this study to determine equilibrium con- are those between 10 and 25 rC by Bonnell and Burridge (1935; upright stants for this reaction between 5 and 22 rC at 0.1 MPa. Rever- triangles), and between 20 and 30 rC by Stout et al. (1966; downward sals were obtained along five humidity-buffer curves. This triangles). The morenosite-retgersite phase boundary based on the technique has been applied to determine the equilibria between thermodynamic data compiled by Wagman et al. (1982) and DeKock 2+ 2+ melanterite [Fe SO4·7H2O] and rozenite [Fe SO4·4H2O] (1982) are represented by the thick dashed and dash-dot lines, respectively. Experimental results obtained in this study are shown by (Chou et al. 2002), chalcanthite [CuSO4·5H2O] and bonattite the large circles along five humidity-buffer cures (near-vertical thin [CuSO4·3H2O] (Chou et al. 2002), goslarite [ZnSO4·7H2O] and bianchite [ZnSO ·6H O] (Chou and Seal 2003), and epsomite solid lines), and the thick solid line is the least-squares fit for new 4 2 experimental data. The equilibrium boundaries for morenosite-saturated [MgSO ·7H O] and hexahydrite [MgSO ·6H O] (Chou and 4 2 4 2 and retgersite-saturated aqueous solutions are shown by the thin dashed Seal, in preparation). It should be emphasized that Reaction 1 and solid curves, respectively (Reardon 1989; personal communication, of this study does not involve an aqueous phase. However, as 2002). These data predict the invariant point for the assemblage will be presented later, in the presence of an additional aque- morenosite + retgersite + aqueous solution + vapor at the invariant ous phase at equilibrium at 0.1 MPa, the system becomes in- temperature of 31.2 rC (Linke and Seidell, 1965; horizontal dotted line) variant with defined equilibrium temperature and humidity. at %RH = 92.0 (open diamond). Our data predict the invariant point at 0 %RH = 95.6, as shown by the solid diamond. For details, see text. The standard Gibbs free energy of reaction, DGr, for Reac- tion 1 was then derived from the equilibrium constant, K, us- ing the relation: EXPERIMENTAL METHOD AND RESULTS 0 Gr =–RT ln K = –RT ln (aH O) = –RT ln (fH O/0.1) = D 2 2 Starting materials were mixtures of reagent grade NiSO4·6H2O (MERCK, T f RH –R ln [( *H2O/0.1) · (% )/100], (2) Lot no.
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