scholarly journals Maghemite in Brazilian Iron Ores: Quantification of the Magnetite-Maghemite Isomorphic Series by Χ-ray Diffraction and the Rietveld Method, and Confirmation by Independent Methods

Minerals ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 346
Author(s):  
Renata Hiraga ◽  
Otávio Gomes ◽  
Reiner Neumann

Maghemite (γ-Fe2O3) is a mineral formed from magnetite oxidation at low temperatures, an intermediate metastable term of the magnetite to hematite oxidation and could be mixed with both. It has magnetic susceptibility similar to magnetite, crystal structure close to magnetite with which it forms a solid solution, while compositionally it equals hematite. Maghemite is thus easily misidentified as magnetite by Χ-ray diffraction and/or as hematite by spot chemical analysis in iron ore characterization routines. Nonstoichiometric magnetite could be quantified in samples of Brazilian soils and iron ores by the Rietveld method using a constrained refinement of the Χ-ray patterns. The results were confirmed by reflected light microscopy and Raman spectroscopy, thus qualitatively validating the method. Χ-ray diffraction with the refinement of the isomorphic substitution of Fe2+ by Fe3+ along the magnetite-maghemite solid solution could help to suitably characterize maghemite in iron ores, allowing for the evaluation of its ultimate influence on mineral processing, as its effect on surface and breakage properties.

Author(s):  
Renata Hiraga ◽  
Otávio da Fonseca Martins Gomes ◽  
Reiner Neumann

Maghemite (γ-Fe2O3) is a mineral formed from magnetite oxidation at low temperatures, an intermediate metastable term of the magnetite to hematite oxidation and could be mixed with both. It has magnetic susceptibility similar to magnetite, crystal structure close to magnetite with which it forms a solid solution, while compositionally it equals hematite. Maghemite is thus easily misidentified as magnetite by X-ray diffraction and/or as hematite by spot chemical analysis in iron ore characterization routines. Nonstoichiometric magnetite could be quantified in samples of Brazilian soils and iron ores by the Rietveld method using a constrained refinement of the X-ray patterns. The results were confirmed by reflected light microscopy and Raman spectroscopy, thus qualitatively validating the method. X-ray diffraction with the refinement of the isomorphic substitution of Fe2+ by Fe3+ along the magnetite-maghemite solid solution could help to suitably characterize maghemite in iron ores, allowing for the evaluation of its ultimate influence on mineral processing, by affecting its surface and breakage properties.


1995 ◽  
Vol 10 (3) ◽  
pp. 189-194 ◽  
Author(s):  
C. L. Lengauer ◽  
G. Giester

The kieserite-type solid-solution series of synthetic (Cu,Mg)SO4·H2O was investigated by TG-analysis and X-ray powder diffraction using the Rietveld method. Representatives with Cu≥20 mol% are triclinic distorted () analogous to the poitevinite (Cu,Fe)SO4·H2O compounds. Cation site ordering with preference of Cu for the more distorted M1 site was additionally proven by the structure refinement.


Author(s):  
K. W. Andrews

In the course of the routine X-ray examination of a number of lowgrade iron ores in order to determine their constitution, it was observed that the calcite phase had varying interplanar spacings. Since these variations could have been due to differing solid-solution contents of other carbonates, further consideration was given to this point. The existence of these generally small amounts of solid solution is of some technological interest.A sample of 'specpure' calcite, supplied by Messrs. Johnson, Matthey & Co. Ltd., was used to provide accurate lattice parameters and interplanar spacings for pure calcite.


2002 ◽  
Vol 17 (5) ◽  
pp. 1112-1117 ◽  
Author(s):  
M. Avdeev ◽  
M. P. Seabra ◽  
V. M. Ferreira

The crystal structure of microwave dielectric ceramics in the (1 − x)La(Mg0.5Ti0.5)O3 (LMT)–xBaTiO3 (BT) (0 ≤ x ≤ 0.9) system has been refined by Rietveld method using x-ray powder diffraction data. LMT and BT were found to form a solid solution in the whole compositional range. The increase of BaTiO3 content results in the following sequence of structure transformations of those solid solutions: P21/n (a−a−c+, B-site ordered) → Pbnm (a−a−c+) → I4/mcm (a0a0c−) → Pm3m (a0a0a0). These structural changes are related to the disappearance of B-site cation ordering (x > 0.1), in-phase tilting (x > 0.3), and antiphase tilting (x > 0.5), respectively.


2004 ◽  
Vol 443-444 ◽  
pp. 353-356
Author(s):  
M. Vennström ◽  
Y. Andersson

Pd3P, which crystallises in the cementite, Fe3C-type structure, forms a solid solution with nickel. The crystal structure contains two crystallographically different palladium sites (8d and 4c). Refinements of neutron powder diffraction intensities using the Rietveld method show that all nickel atoms occupy the eight-fold position. The unit cell parameters were refined to a=5.7812(4) Å, b=7.4756(6) Å and c=5.1376(4) Å, for Pd2.7Ni0.3P0.94.


2008 ◽  
Vol 8 (4) ◽  
pp. 2029-2036 ◽  
Author(s):  
W. Tebib ◽  
S. Alleg ◽  
R. Bensalem ◽  
N. Bensebaa ◽  
F. Z. Bentayeb ◽  
...  

Nanostructured Fe-8P (wt%) powder mixture was prepared by high energy ball milling in a planetary ball mill (Fritsch P7) under argon atmosphere. The morphology of the particles, the phase identification and the alloying evolution process as a function of milling time are studied by scanning electron microscopy (SEM), X-ray diffraction (XRD) and 57Fe Mössbauer spectrometry (MS), respectively. Refinement based on Rietveld method of the XRD patterns and the Mössbauer spectra analysis show that the FexP (1 < x < 2) and Fe2P phosphide phases are the main product after 3 h of milling (∼10%). From the XRD Rietveld refinement, it is observed that the Fe2P phase disappears completely after 12 h of milling, while the Fe3P nanophase appears after 9 h and remains for larger milling duration. The lattice structure distortion is evidenced by the lattice parameter changes ofthe milled products. A two structure state of the α-Fe(P) solid solution: α-Fe1 and α-Fe2 is confirmed by both the XRD and MS measurements. After milling for 21 h, a mixture of a disordered two phase α-Fe(P) solid solution, Fe3P nanophase and a small amount of a paramagnetic FeP phosphide phase (∼2%) is obtained.


2020 ◽  
Vol 58 (2) ◽  
pp. 203-221
Author(s):  
Emil Makovicky ◽  
Sven Karup-Møller

ABSTRACT The central portions of the condensed phase system Cu–Fe–Se were investigated by means of dry syntheses in evacuated silica glass tubes at 900, 750, 600, 500, 450, 350, and 300 °C. Synthesis products were studied by reflected-light microscopy and electron microprobe analyses. The field of sulfide melt is extensive at 900 °C and retreats progressively towards the Cu–Se side at 750 °C; residual selenide melt persists at 600 °C. The selenium analogue of iss was found only at and below 600 °C; eskebornite becomes individualized at and below 500 °C, whereas the selenium analogue of bornite solid solution is present at all investigated temperatures, although with reduced extent on temperature decrease. The three iron selenides (β, γ, δ) display considerable solubility of copper, which for the mackinawite-like β FeSe reaches 14 at.% Cu at 300 °C. FeSe2 displays an immiscibility gap with isotropic solid solution (Cu,Fe)Se2, the composition of which gradually changes towards Cu-rich with decreasing temperature. Similarities and differences with the sulfur-based system are highlighted.


2003 ◽  
Vol 67 (5) ◽  
pp. 957-965 ◽  
Author(s):  
E. P. Reguir ◽  
A. R. Chakhmouradian ◽  
R. H. Mitchell

AbstractSome samples of hollandite-type titanates from the Murun alkaline complex (Yakutia, Russia) contain appreciable amounts of Pb (up to 12.5 wt.% PbO). These titanates occur in a pegmatitic K-feldsparaegirine rock containing subordinate K-rich batisite, titanite, wadeite and other minerals. The Pb-bearing crystals coexist with hollandite-type phases devoid of detectable Pb and zoned from a Kdominant (priderite) core to a Ba-dominant (henrymeyerite) rim. Recalculation of the microprobe analyses on the stoichiometric basis indicates that most of the Fe occurs in this mineral in trivalent form, suggesting the existence of a solid solution between the Ba(Ti6Fe)O16, K2(Ti6Fe)O16 and Pb(Ti6Fe)O16 end-members. The maximum proportion of the latter end-member in the Murun titanates is ∽45 mol.%. The Ba-free compositions [Pb1.0–1.3(Ti,Fe)8O16] and intermediate members of the (Ba1–xPbx)(Ti6Fe)O16 series were synthesized at 1050 –1100ºC. The synthesis products comprise tetragonal hollandites of various stoichiometry intermixed with rutile, a pseudobrookite-type phase and (for the Ba-free compositions) minor macedonite. Electron microprobe analyses of the hollandites indicate that there is a continuous series of compositions between the two hexatitanate end-members, Ba(Ti6Fe)O16 and Pb(Ti6Fe)O16. The crystal structure of one intermediate member was refined by the Rietveld method in space group I4/m, and found to differ from the hollandite archetype (i.e. Pb-bearing Ba manganate) in that Pb is preferentially partitioned into the 2b tunnel site at (0,0,½), whereas Ba is partitioned into the larger 4e site at (0,0,∽0.8).


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