THE MOSSBAUER SPECTRA OF HYDROXYCARBONATE GREEN RUSTS

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1 Clay Minerals (1984) 19, THE MOSSBAUER SPECTRA OF HYDROXYCARBONATE GREEN RUSTS E. MURAD AND R. M. TAYLOR* Lehrstuhl fiir Bodenkunde, Technische Universitdt Mffnchen, D-85 Freising-Weihenstephan, Federal Republic of Germany, and *CSIRO Division of Soils, Private Bag 2, Glen Osmond, South Australia 564 (Received 29 July 1983) A B S T R A C T: M6ssbauer spectra of Fe2+Fe 3+ and Fe2+A1 hydroxycarbonates taken in the paramagnetic state were fitted using two Fe 2+ and Fe 3+ doublets each. These spectra can be interpreted in terms of an ordered cation arrangement in the pyroaurite-type structure. The inner Fe 2+ doublet seems to be the outcome of excess Fe 3+ in the samples studied. The outer Fe 2+ doublet (quadrupole splitting ~2.8 mm s -1, FWHM =.26 mm s -l) is relatively well-defined and can, together with the fact that this doublet disappears on oxidation, possibly serve to identify these compounds in natural systems. Green rusts of the Fe2+(Fe3+,A1)-hydroxycarbonate type have crystal structures resembling that of pyroaurite (Stampfl, 1969; Taylor, 198). The structures of these compounds consist of Fe 2+ and Fe 3+ and/or A13+ ions octahedrally surrounded by oxygen in brucite-like sheets that are approximately 7.8 A apart, and separated by interlayers containing CO ]- and H2. The formulae of such green rusts can, by analogy to that of pyroaurite, be written (Fe3+,A1)2Fe2+(OH)L6CO3.4H2. The Fe2+/Fe 3+ ratio may, however, vary somewhat, and can be as low as 2:1 (Stampfl, 1969; Allmann, 197; Taylor, 1973). Carbonate-containing green rust has been identified as a corrosion product in municipal water pipes by Stampfl (1969). Green rusts could also be constituents of those hydromorphic soils which can be observed to change colour on exposure to the atmosphere--often within a matter of minutes--from bluish-green to brown. This instability towards oxidation has so far prevented the identification of green rusts in nature, because it renders the application of standard techniques of soil mineral analysis, such as X-ray diffraction, difficult. The importance of these compounds in soils should, however, not be underestimated a priori. Green rusts are probably precursors of different iron oxides found in soils, which may have formed directly by oxidation of these, or indirectly via other, intermediate phases (Schwertmann & Taylor, 1977). In the present paper the M6ssbauer spectra of Fe2+Fe 3+ and Fe2+A1 green rusts are described, with a view to providing information which may eventually help identify these compounds in nature. MATERIALS AND METHODS One Fe2+Fe 3+ green rust (sample 81/48) and one Fe2+A1 green rust (sample 81/49) were prepared using the technique of Taylor & McKenzie (198) and Taylor (198), modified The Mineralogical Society

2 78 E. Murad and R. M. Taylor as described by Taylor (1982). To prevent oxidation, the samples were kept frozen under dry ice prior to M6ssbauer analysis. The M6ssbauer spectrometer comprised a 57Co/Rh source driven in a sinusoidal mode. Spectra were taken in a bath cryostat, at ~ 12 K under a He atmosphere and at 4.2 K by immersion in liquid He, with both source and absorber kept at the same temperature. Data were accumulated in a 124-channel analyser and processed using a CDC Cyber 175 computer. Component lines of doublets were constrained to have equal widths and intensities. A 6-pro iron foil served for velocity calibration and as the isomer shift reference. RESULTS The 12 K M6ssbauer spectrum of the Fe2+Fe 3+ hydroxycarbonate (W81/48)is adequately fitted by four doublets (Fig. l a). Two each of these doublets can be assigned to Fe 2+ (D1 and D2) and Fe 3 (D3 and D4 in Table 1 and Fig. la). The Fe 2+ doublets have similar isomer shifts (/Fe = 1.14 mm s -1) but different quadrupole splittings (AEQ = 2.89 and 2.23 mm s-l); the Fe 3 doublets likewise (/Fe =.38; AEQ =.49 and.95 mm s-l). Of the Fe 2+ doublets, the outer one (D 1) has narrower lines than the inner one (D2:.26 vs.4 mm s-l), and a higher relative intensity (.4 vs.27). Following measurement of the spectra, the sample was exposed for 2 h to the atmosphere at room temperature. This resulted in a colour change from olive-green to brown. The 12 K M6ssbauer spectrum of this oxidized sample (Fig. lb) could be satisfactorily fitted with one Fe 2+ doublet (D2' in Table 1 and Fig. lb) and two Fe 3+ doublets (D3' and D4'). The isomer shift values (averaging 1.12 mm s -~ for Fe z+ and.37 mm s -~ for Fe 3+) are not affected by the oxidation. The quadrupole splitting of the remaining Fe 2+ doublet (2.39 mm s -~) was only slightly larger than that of D2 in the original sample (2.23 mm s-l), but the line width increased from.4 to -5 mm s -~. The parameters of the Fe 3+ components (c~/fe =.37 mm s-l; AE o =.63 and 1.2 mm s -l) are similar both to those of Fe 3+ in the original sample (W81/48) and those observed for superparamagnetic ferrihydrite (Childs & Johnston, 198; Murad & Schwertmann, 198). The relative intensities of the Fe a+ components have errors an order of magnitude larger than those of the original sample (see Table 1). The 12 K M6ssbauer spectrum of the Fe2+AI hydroxycarbonate W81/49 was fitted with two Fe 2+ doublets and one Fe 3+ doublet (Fig. lc). The isomer shifts of all components of this spectrum were the same as for the Fe2+Fe 3+ hydroxycarbonate W81/48. The outer Fe 2+ doublet also had essentially the same quadrupole splitting as W81/48, whereas the quadrupole splitting of the inner doublet bore more resemblance to that of the oxidized Fe2+Fe 3 sample. The relative intensity of the Fe 3+ doublet was somewhat lower than observed for Fe 3 in W81/48 (.2 vs.33). These results may be compared to room-temperature M6ssbauer spectra of two green rusts formed by corrosion of metallic iron with NHaNO a (Gancedo et al., 1976). The spectra of these samples were each resolved into only one Fe 2+ doublet (AE e 2.3 and 2.37 mm s -1) and a very broad (FWHM ~.8 mm s -1) single-line Fe 3 component. The Fe2+/Fe 3 ratios deduced from these spectra (1.9 and 2.6) were, however, quite similar to that found for W81/48 (2.). Analysis of 4.2 K M6ssbauer spectra run on the original and oxidized sample W81/48 is complicated by the fact that these show partial (4% of the total area) and complete

3 MSssbauer spectra of green rusts 79 ~ oo ~ o DI[ E' "" a 5 "S CO o. CO Z ~ o w8~/49 t ~" ' CO I I I I, -2. VELOCI TY I 9 21, HH/SEC) ~12K 4L. O FIo. 1. M6ssbauer spectra of (a) Fe2+Fe 3+ hydroxycarbonate initially and (b) after two hours' exposure to the atmosphere, and (c) Fe2+A1 hydroxycarbonate. All spectra taken at ~12 K; bars marked D 1, D2 etc. indicate positions of component doublets.

4 8 E. Murad and R. M. Taylor TABL~ 1. M6ssbauer parameters of hydroxycarbonate green rusts at 12 K. Spectral 6(Fe) AEQ FWHM Sample no. component (mm s -1) (mm s -1) (mm s-l) /relative W81/48 D (1) 2-89 (1).26 (1).4 (1) (1) 2.23 (1).4 (1) -27 (1) D3.36 (1).49 (1).28 (I).24 (1) D4.4 (1).95 (3).35 (4).9 (1) W81/48 DE' 1.1 (2) 2.39 (5).5 (2).24 (3) Ox D3'.37 (1).63 (1).37 (1).4 (1) D4'.37 (I) 1.2 (5).37 (2).3 (2) W81/49 D (1) 2.84 (1).26 (2).3 (1) DE 1.13 (1) 2.48 (2).32 (1).5 (9) D3/4.37 (1).63 (1).37 (2).2 (4) ~(Fe) = isomer shift relative to metallic iron. AEQ = quadrupole splitting. FWHM = full line width at half maximum. Numbers in parentheses give standard deviation on last digit. magnetic ordering, respectively. The 4.2 K spectrum of W81/48 shows paramagnetic doublets which can be assigned to Fe 2+ and Fe 3+. The magnetically ordered portion of this spectrum seems to be complex (i.e. containing components of Fe E+ and Fea+); the spectrum of the oxidized sample W81/48 can be fitted with one sextet that has a magnetic hyperfine field of 48 koe and broad lines of 1.2 mm s -1. DISCUSSION The results can be best understood if an ordered distribution of Fe 2+ and Fe 3+ and a ratio of 3 : 1 for Fe2+/Fe 3+ are assumed for a stoichiometric (i.e. an Fe]+Fe ~+) hydroxycarbonate. Such a distribution is shown schematically in Fig. 2. In this case there will be only one crystallographic site (i.e. lattice position with identical neighbours) each for Fe 2+ and Fe 3+, and the Mtssbauer spectrum should show one component for each of these, with an intensity ratio of 3 : 1. Substitution of Fe 3+ for Fe 2+ on an Fe 2+ site will modify this regular structure. Such a substitution can be either inherent (due to excess Fe 3+ in the original precipitate) or result from subsequent oxidation of an initially 3:1 green rust. Exposure of Fe2+Fe a+ hydroxycarbonates to the atmosphere results in a rapid oxidation of Fe 2+. X-ray diffraction indicates thai the structure is preserved at least during the initial stages of oxidation; the lattice spacings, however, being reduced as Fe 2+ ions are oxidized to form smaller Fe 3+ ions (Taylor, 198; 1982). The replacement of one Fe 2+ ion by Fe 3+ (Fig. 2; cross-hatched circle in second row from top) can be seen to have identical effects on two neighbouring Fe 2+ ions with which the oxidized ion shares octahedral edges, and seven more remote Fe 2+ ions with which it shares corners. The Fe 2+ ions will consequently be in an environment different from that in a stoichiometric 3:1 Fe2+Fe 3+ green rust, and the electric field gradient at these sites will differ from the original one. The spectral components for an unoxidized 3 : 1 Fe2+Fe 3+ hydroxycarbonate seem to be given by the doublets D1 and D3 in the M6ssbauer spectrum of W81/48 (Fig. la and

5 M6ssbauer spectra of green rusts 81 FIG. 2. Model of the brucite sheet in the Fe2+Fe 3+ hydroxycarbonate showing an ordered arrangement of Fe 2+ (open circles) and Fe 3+ (closed circles). Cross-hatching indicates an ideally Fe 2+ ion replaced by Fe3+; hatched circles show different orientations of Fe 2+ with respect to such an oxidized ion. Table 1). The existence of the Fe 2+ doublet D2 and the Fe 3+ doublet D4 can be attributed to excess Fe 3+ (relative area.33 instead of theoretically.25) in this sample. As the sample oxidizes, the Fe3+/Fe 2+ ratio (and correspondingly the relative intensity of the Fe J+ components in the M6ssbauer spectrum) will increase. The intensities of the Fe 2+ and Fe 3+ components in W81/48 and W81/48 (oxidized) show that two hours' exposure to the atmosphere had reduced the Fe2+/Fe 3+ ratio of this sample from 2:1 to about 1:3. The doublet D 1 of the original sample has disappeared, and the quadrupole splitting of the remaining Fe 2+ doublet, D2', is similar to that of doublet D2 in the original sample. As oxidation increases, there will be an increasing probability for two newly formed Fe a+ ions to become neighbours, sharing either oetahedral edges or corners. It is obvious that this will create a variety of environments for the remaining Fe 2 ions that will differ not only from those of the original Fe 2+ ions, but also from those in only weakly oxidized samples (e.g. W81/48; cf. hatched and cross-hatched circles in fourth row from top in Fig. 2). This may explain the somewhat different quadrupole splitting of D2' compared to D2 in samples W81/48 (oxidized) and W81/48, respectively, and the large line width of D2'. An Fe 3+ ion formed by oxidation of Fe 2+ (cross-hatched circles in Fig. 2) will not only be in an environment that differs from that of the originally present Fe 3+, but will also affect the environments of neighbouring Fe 3+ ions. As oxidation proceeds, more Fe 3+ ions will be formed from Fe 2+, resulting in numerous possible environments both for these and

6 82 E. Murad and R. M. Taylor the original ions (Fig. 2, bottom hatched circles). A statistically satisfactory (though possibly simplified) fit of the Fe 3+ components of such an oxidized sample (Fig. lb) can be carried out using two doublets of different quadrupole splittings (D3' and D4' in Table 1). The existence of the weak Fe 3+ doublet D4 in the original sample W81/48 indicates that this may have experienced incipient oxidation. The Fe2+A1 hydroxycarbonate W81/49 can be referred to the same structural model used to characterize the Fe2+Fe 3+ compound (Fig. 2), with A1 replacing Fe 3+. This again leads to the expectation of one Fe 2+ doublet, corresponding to that expected for the Fe2+Fe 3+ hydroxycarbonate, but no Fe 3+ component. Provided all the Fe 3+ is replaced by A1 in the unoxidized state, any Fe 3+ detected in the M6ssbauer spectrum should be the outcome of oxidation. The M6ssbauer spectrum of sample W81/49, i.e. the studied Al-member of the hydroxycarbonate series, shows, however, a significant contribution of Fe 3+ (2% of the total area under the 12 K spectrum), and a ratio of areas under the Fe 2+ doublets D1 and D2 of.6 : 1. It is conceivable that due to excess Fe 2+ in the system, some will be oxidized in solution, so that the final product could well be a Fe2+(Fe3+AI) hydroxycarbonate rather than the pure Fe2+A1 end-member. Some Fe a+ may also result from oxidation of Fe 2+ after crystallization of the sample. The oxidation of this sample could result from a smaller particle size, making it more susceptible to oxidation than W81/48. Due to the poorer counting statistics of this spectrum compared to that of W81/48, only one Fe 3+ doublet could be fitted to the data. The structural model depicted in Fig. 2 is in apparent contradiction to X-ray diffraction work by Allmann (1968) on pyroaurite, which indicated random distribution of Mg and Fe a in the octahedral sheets. Cation ordering in minerals of this group has, however, been observed in pyroaurite and the 2H-polytype sj6grenite (Taylor, 1969) and the synthetic MgAI hydroxycarbonates (Gastuche et al., 1967). It thus seems possible that cation ordering may also take place in the Fe2+Fe 3+ and Fe2+A1 hydroxycarbonates, especially in view of the large ionic radius of Fe 2+ (- 74 A, in contrast to.66 A for Mg2 The narrow lines (FWHM.26 mm s -1) of the outer Fe 2+ doublets D1 in the M6ssbauer spectra of both W81/48 and W81/49 indicate that these doublets result from a site with a well-defined electric field gradient (rather than a distribution of field gradients, which would be more likely if the occupancy of the cation sites were random). On oxidation, new Fe a+ sites will be created. The effects of these have been discussed above. CONCLUSIONS M6ssbauer spectra of Fe2+Fe a+ and Fe2+A1 hydroxycarbonates ('green rusts') in which the cations are ordered should ideally comprise one Fe 2+ doublet with a quadrupole splitting of about 2.8 mm s-l; the Fe2+Fe 3+ compound also has an Fe 3+ doublet. The observation here of two Fe 2+ and Fe 3+ doublets of different quadrupole splittings can be explained in terms of excess Fe 3+. During oxidation the total area of the Fe 3+ spectral components increases at the cost of the Fe 2+ components, the Fe 2+ doublet with narrow lines and quadrupole splitting of 2.8 mm s -1 disappearing first. In soils, other constituents, notably clay minerals, have M6ssbauer spectra with similar parameters (Heller-Kallai & Rozenson, 1981). Spectra of unoxidized or partly oxidized green rusts may therefore not be specific in natural systems. A significant increase in Fe 3+ spectral components at the cost of Fe 2+ following some hours' exposure to the atmosphere

7 M~ssbauer spectra of green rusts 83 will, however, indicate the presence of such compounds. Stripping procedures, in which the spectra of the oxidized samples are subtracted from spectra of the unoxidized samples, may reveal the parameters of the Fe 2+ components, thus making a more definitive identification possible. ACKNOWLEDGMENTS We are indebted to F. E. Wagner for making the M6ssbauer measurements at the Physics Department oft. U. MiJchen possible, to R. Allmann for a helpful discussion, and to L. H. Bowen and U. Schwertmann for constructive reviews of the manuscript. Thanks are also extended to L. H. Bowen for making the services of the North Carolina State University of Raleigh available while we were writing up this paper, to Joyce Weatherspoon who typed several drafts of the manuscript, and to the Deutsche Forschungsgemeinschaft and the Deutscher Akademischer Austauschdienst for financial support. REFERENCES ALLMANN R. (1968) The crystal structure of pyroaurite. Acta Cryst. B24, ALLMANN R. (197) Doppelschichtstrukturen mit brucit~ihnlichen Schichtionen [Me(II)l_xMe(III)x(OH)2] x+. Chimia 24, CHILDS C.W. & JOHNSTOr~ J.H. (198) M6ssbauer spectra of proto-ferrihydrite at 77 K and 295 K, and a reappraisal of the possible presence of akagan6ite in New Zealand soils. AustraL J. Soil Res. 18, GANCEDO J.R., MAarrNEZ M.L. & OTON J.M. (1976) M6ssbauer spectroscopy study of corrosion products of iron with ammonium nitrate in aqueous solutions. J. Physique 37 C6, GASTtJCnE M.C., BROWN G. & MORTLAND M.M. (1967) Mixed magnesium-aluminium hydroxides. I. Preparation and characterization of compounds formed in dialysed systems. Clay Miner. 7, HELLER-KALLAI L. & ROZENSON I. (1981) The use of M6ssbauer spectroscopy of iron in clay mineralogy. Phys. Chem. Miner. 7, MURAD E. & SCrtWER~A~n~ U. (198) The M6ssbauer spectrum of ferrihydrite and its relations to those of other iron oxides. Am. Miner. 65, SCt-IWF.Ra~A~ U. & TAYLOR R.M. (1977) Iron oxides. Pp in: Minerals in SoilEnvironments (J.B. Dixon & S.B. Weed, editors). Soil Science Society of America, Madison, WI. STAIVlPFL P.P. (1969) Ein basisches Eisen-II-III-Karbonat in Rost. Corrosion Sci. 9, TAYLOR H.F.W. (1969) Segregation and cation-ordering in sj6grenite and pyroaurite. Mineral. Mag. 37, TAYLOR H.F.W. (1973) Crystal structures of some double hydroxide minerals. Mineral. Mag. 39, TAYLOR R.M. (198) Formation and properties of Fe(II)Fe(IIl) hydroxy-carbonate and its possible significance in soil formation. Clay Miner. 15, TAYLOa R.M. (1982) Stabilization of eolour and structure in the pyroaurite-type compounds Fe(II)Fe(III)Al(III)-hydroxycarbonates. Clay Miner. 17, TAYLOR R.M. & MCKENzm R.M. (198) The influence of aluminum on iron oxides. VI. The formation of Fe(II)-AI(III) hydroxy-chlorides, -sulfates, and -carbonates as new members of the pyroaurite group and their significance in soils. Clays Clay Miner. 28,

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