Hostname: page-component-78c5997874-v9fdk Total loading time: 0 Render date: 2024-11-19T03:22:19.439Z Has data issue: false hasContentIssue false
  • English
  • Français

Synthesis and Rietveld crystal structure refinement of mackinawite, tetragonal FeS

Published online by Cambridge University Press:  05 July 2018

A. R. Lennie ,
S. A. T. Redfern ,
P. F. Schofield  and
D. J. Vaughan
A. R. Lennie
Affiliation:
Department of Earth Sciences, The University of Manchester, Oxford Road, Manchester, M13 9PL, UK
S. A. T. Redfern
Affiliation:
Department of Earth Sciences, University of Cambridge, Downing Street, Cambridge, CB2 3EQ, UK
P. F. Schofield
Affiliation:
Department of Mineralogy, The Natural History Museum, Cromwell Road, London, SW7 5BD, UK
D. J. Vaughan
Affiliation:
Department of Earth Sciences, The University of Manchester, Oxford Road, Manchester, M13 9PL, UK
Get access Rights & Permissions [Opens in a new window]

Abstract

Mackinawite, tetragonal FeS, has been synthesised by reacting iron with Na2S solutions. A Rietveld structure refinement of X-ray powder diffraction data, recorded using X-rays monochromated from synchrotron radiation with a wavelength of 0.6023 Å, has been performed. The structure has been refined in the tetragonal space group, P4/nmm, and has the following cell parameters: a = 3.6735(4), c = 5.0328(7) Å, V = 67.914(24) Å3. Our refinement shows that the FeS4 tetrahedron in mackinawite is almost perfectly regular, with a much smaller distortion than has been previously reported. An improved X-ray diffraction data set is provided.

Keywords

mackinawiteRietveld structure refinementsynthesis
Type
Experimental Mineralogy
Information
Mineralogical Magazine , Volume 59 , Issue 397 , December 1995 , pp. 677 - 683
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 1995

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Berner, R.A. (1962) Tetragonal FeS, a new iron sulfide. Science, 137, 669.CrossRefGoogle Scholar
Berner, R.A. (1964) Iron sulfides formed from aqueous solution at low temperatures and atmospheric pressure. J. Geol., 72, 293–306.CrossRefGoogle Scholar
Bertaut, E.F., Burlet, P. and Chappert, J. (1965) Sur 1'absence d'ordre magnetique dans la forme quad-ratique de FeS. Solid State Comm., 3, 335–8.CrossRefGoogle Scholar
Clark, A.H. (1966) Some comments on the composition and stability relations of mackinawite. Neues Jahrb. Mineral, Mh., 300-4.Google Scholar
Davison, W. (1991) The solubility of iron sulphides in synthetic and natural waters at ambient temperature. Aquatic Sciences, 53/4, 309–29.CrossRefGoogle Scholar
Evans, H.T. Jr, Berner and , R.A. & Milton, C. (1962) Valleriite and mackinawite. Geol. Soc. America Program 1962, Annual Meeting, 47a.Google Scholar
Evans, H.T. Jr., Milton, C, Chao, E.C.T., Adler, I., Mead, C, Ingram, B. and Berner, R.A. (1964) Valleriite and the new iron sulfide, mackinawite. U.S. Geol. Surv. Prof. Pap., 475-D, 64-9.Google Scholar
Grnvold, F. (1968) Heat capacities and thermodynamic properties of the iron selenides Fe104Se, FeySg and Fe3Se4 from 298 to 1050°K. Ada Chem. Scand., 22, 1219–40.CrossRefGoogle Scholar
Grnvold, F. and Westrum, E.F. Jr. (1959) Low temperature heat capacities and thermodynamic properties of the iron selenides Fe104Se, Fe7S8 and Fe3Se4 from 5 to 350°K. Ada Chem. Scand., 13, 241-8.CrossRefGoogle Scholar
Grnvold, F., Haraldsen, H. and Vihovde, J. (1954) Phase and structural relations in the system iron-tellurium. Ada Chem. Scand., 8, 1927–42.CrossRefGoogle Scholar
Hagg, G. and Kindstrom, A.L. (1933) Rontgenuntersu-chung am System Eisen-Selen. Z. physik. Chem., B, 22, 453–64.Google Scholar
Haraldsen, H., Grnvold, F. and Vihovde, J. (1944) Faseforholdene i systemet jern-tellur. Tidsskrf. Kjemi Bergv., 4, 96–8.Google Scholar
Hoffmann, R. (1988) Solids and surfaces: A chemist's view of bonding in extended structures. VCH.CrossRefGoogle Scholar
Kuovo, O., Vuorelainen, Y. and Long, J.V.P. (1963) A tetragonal iron sulfide. Amer. Mineral., 48, 511–24.Google Scholar
Lennie, A.R. (1994) Aspects of relations between metastable and stable phases in the iron-sulphur system. Unpublished PhD thesis, University of ManchesterGoogle Scholar
Meyer, F.H., Riggs, O.L., McGlasson, R.I. and Sudbury, J.D. (1958) Corrosion products of mild steel in hydrogen sulfide environments. Corrosion, 14, 109-15.Google Scholar
Murray, A.D., Cockroft, J.K. and Fitch, A.N. (1990) Powder Diffraction Program Library (PDPL). University College, London.Google Scholar
Sarkar, S.C. (1971) Mackinawite from the sulfide ores of the Singhbhum Copper belt, India. Amer. Mineral., 56, 1312–18.Google Scholar
Takeno, S. (1965a) A note on mackinawite (so-called valleriite) from the Kawayama mine. Japan. Geol. Rept. Hiroshima Univ., 14, 59–76.Google Scholar
Takeno, S. (1965b) Thermal studies on mackinawite. J. Sci. Hiroshima Univ. Ser. C, 4, 455–78.Google Scholar
Takeno, S. and Clark, A.H. (1967) Observations on tetragonal (Fe, Ni, Co)1+xS, mackinawite. J. Sci Hiroshima Univ. Ser. C, 5, 287–93.Google Scholar
Takeno, S., Moh, G.H. and Wang, N. (1982) Dry mackinawite syntheses. Neues Jahrb. Mineral., Abh., 144, 291–342.Google Scholar
Taylor, L.A. and Finger, L.W. (1970) Structural refinement and composition of mackinawite. Carnegie Institute of Washington Geophys. Lab. Ann. Rept., 69 318-22.Google Scholar
Tsuji, T., Howe, A.T. and Greenwood, N.N. (1976) The Fe—Se system. I. Mossbauer spectra and electrical conductivity of Fe! 04Se. J. Solid State Chem., 17, 157-63.CrossRefGoogle Scholar
Uda, M. (1968) The structure of tetragonal FeS. Z. anorg. Chem., 361, 94–8.CrossRefGoogle Scholar
Vaughan, D.J. and Craig, J.R. (1978) Mineral chemistry of metal sulfides. Cambridge University Press.Google Scholar
Yamaguchi, S. and Moori, T. (1972) Electrochemical synthesis of ferromagnetic Fe3S4 . J. Electrochem. Soc, 119, 1062.CrossRefGoogle Scholar
Zôka, H., Taylor, L.A. and Takeno, S. (1972) Compositional variations in natural mackinawite and the results of heating experiments. J. Sci. Hiroshima Univ., Ser. C, 7, 37–53.Google Scholar