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Crystal structure and formula revision of deliensite, Fe[(UO2)2(SO4)2(OH)2](H2O)7
- J. Plášil, J. Hauser, V. Petříček, N. Meisser, S. J. Mills, R. Škoda, K. Fejfarová, J. Čejka, J. Sejkora, J. Hloušek, J.-M. Johannet, V. Machovič, L. Lapčák
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- Mineralogical Magazine / Volume 76 / Issue 7 / December 2012
- Published online by Cambridge University Press:
- 05 July 2018, pp. 2837-2860
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The crystal structure of deliensite, Fe[(UO2)2(SO4)2(OH)2](H2O)7, was solved by direct methods and refined to R1 = 6.24% for 5211 unique observed reflections [Iobs > 3σ(I)], on a crystal that was found to consist of rotational and inversion (merohedral) twins, from Jeroným mine, Abertamy in the Czech Republic. The presence of four twin domains was taken into account in the refinement. The structure is orthorhombic, space group Pnn2, with unit-cell parameters a = 15.8514(9), b = 16.2478(7), c = 6.8943(3) Å, V = 1775.6(1) Å3 and Z = 4. The crystal structure of deliensite contains uranyl-sulfate sheets with a phosphuranylite topology, consisting of dimers of edge-sharing uranyl pentagonal bipyramids linked by corner-sharing with sulfate tetrahedra. The sheets lie in the (100) plane and are decorated by [Fe2+O(H2O)5] octahedra; two weakly bonded H2O molecules are present in the interlayer. The [Fe2+O(H2O)5] octahedron is linked directly to the sheet via the uranyl oxygen atom. Adjacent sheets are linked by hydrogen bonds only. The sheet topology and geometrical isomerism is discussed and a comparison of the composition obtained from electron-probe microanalysis, powder-diffraction data, Raman and infrared spectra of deliensite samples from Mas d'Alary, Lodève, France; L'Ecarpière mine, Gétigné, France; and several localities at Jáchymov, Western Bohemia, Czech Republic is made.
Štěpite, U(AsO3OH)2·4H2O, from Jáchymov, Czech Republic: the first natural arsenate of tetravalent uranium
- J. Plášil, K. Fejfarová, J. Hloušek, R. Škoda, M. Novák, J. Sejkora, J. Čejka, M. Dušek, F. Veselovský, P. Ondruš, J. Majzlan, Z. Mrázek
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- Journal:
- Mineralogical Magazine / Volume 77 / Issue 1 / February 2013
- Published online by Cambridge University Press:
- 05 July 2018, pp. 137-152
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Štěpite, tetragonal U(AsO3 OH)2(H2O)4 (IMA 2012-006), is the first natural arsenate of tetravalent uranium. It occurs in the Geschieber vein, Jáchymov ore district, Western Bohemia, Czech Republic, as emerald-green crystalline crusts on altered arsenic. Associated minerals include arsenolite, běhounekite, claudetite, gypsum, kaatialaite, the new mineral vysokýite (IMA 2012-067) and a partially characterized phase with the formula (H3O)+2(UO2)2(AsO4)2˙6H2O. Štěpite typically forms tabular crystals with prominent {001} and {010} faces, up to 0.6 mm in size. The crystals have a vitreous lustre and a grey to greenish grey streak. They are brittle with an uneven fracture and a very good cleavage on (001). Their Mohs hardness is about 2. Štěpite is not fluorescent in either short-wave or long-wave ultraviolet light. It is biaxial (–) with refractive indices (at 590 nm) of α = 1.636(2), β = 1.667(3), γ = 1.672(2) and 2Vobs < ~5°, anomalous greyish to pale yellow interference colours, and no pleochroism. The composition is as follows: 0.12Na2O, 50.19 UO2, 0.04SiO4, 0.09 P2O5, 0.93 As2O5, 1.95 SO3, 16.41 H2O; total 107.90 wt.%, yielding an empirical formula (based on 12 O a. p. f. u.) of (U1.01Na0.02)Σ1.03[(AsO3OH)1.82 (PO3OH)0.04(SO4)0.13(SiO4)0.01]Σ 2.00˙4H2O. Štěpite is tetragonal, crystallizing in space group I41/acd, with a = 10.9894(1), c = 32.9109(6) Å, V = 3974.5(1) Å3, Z = 16 and Dcalc = 3.90 g cm-3. The six strongest peaks in the X-ray powder-diffraction pattern [dobs in Å (I) (hkl)] are as follows: 8.190(100)(004), 7.008(43)(112), 5.475(18)(200), 4.111(16)(008), 3.395(20)(312,217), 2.1543(25)(419). The crystal structure of šteěpite has been solved from singlecrystal X-ray diffraction data by the charge-flipping method and refined to R1 = 0.0353 based on 1434 unique observed reflections, and to wR2 = 0.1488 for all 1523 unique reflections. The crystal structure of štšpite consists of sheets perpendicular to [001], made up of eight-coordinate uranium atoms and hydroxyarsenate 'tetrahedra'. The ligands surrounding the uranium atom consist of six oxygen atoms which belong to the hydroxyarsenate groups and two oxygen atoms which belong to interlayer H2 O molecules. Each UO8 polyhedron is connected to five other U polyhedra via six AsO3OH groups. Adjacent electroneutral sheets, of composition [U4+(AsO3OH)22-]0, are linked by hydrogen bonds involving H2 O molecules in the interlayers and OH groups in the sheets. The new mineral is named in honour of Josef Štěp (1863–1926), a Czech mining engineer and 'father' of the world's first radioactive spa at Jáchymov.
Widenmannite, a rare uranyl lead carbonate: occurrence, formation and characterization
- J. Plášil, J. Čejka, J. Sejkora, P. Škácha, V. Goliáš, P. Jarka, F. Laufek, J. Jehlička, I. Němec, L. Strnad
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- Mineralogical Magazine / Volume 74 / Issue 1 / February 2010
- Published online by Cambridge University Press:
- 05 July 2018, pp. 97-110
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The rare uranyl lead carbonate widenmannite, Pb2(UO2)(CO3)3, was found at the Jánská vein, Příbram, Czech Republic, where two generations occur in several morphological types and mineral associations in hydrothermal veins. Alpha spectroscopy shows that these two generations have different ages, >220,000 and 118±12 y. ICP-MS analysis indicates that both widenmannites have a dominance of non-radiogenic Pb which originates from weathered galena. The older widenmannite I forms fine-grained, grey to beige aggregates in the highly altered supergene part of the hydrothermal ore vein in association with pyromorphite, cerussite and goethite. The younger widenmannite II occurs as white, yellow or greenish-yellow thin tabular crystals upto 0.5 mm long in association with cerussite, anglesite, limonite, kasolite and an unnamed Pb-U-O phase. Thermal analysis suggests that widenmannite decomposes in several steps, with Pb uranate as the final product. Infrared and Raman spectroscopy confirm the presence of non-equivalent (CO3)2– groups, bidentately coordinated in uranyl hexagonal polyhedra, forming the well known uranyl tricarbonate complex. Infrared spectroscopy shows conclusively that widenmannite does not contain molecular H2O.
The crystal structure of rabejacite, the Ca2+-dominant member of the zippeite group
- J. Plášil, M. Dušek, J. Čejka, J. Sejkora
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- Mineralogical Magazine / Volume 78 / Issue 5 / October 2014
- Published online by Cambridge University Press:
- 05 July 2018, pp. 1249-1264
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The crystal structure of rabejacite from Jáchymov, ideally Ca2[(UO2)4O4(SO4)2](H2O)8, was solved by charge flipping from single-crystal data and refined to R1 = 11.94% for 1422 unique observed reflections [I > 3σ(I)]. According to single-crystal X-ray data, rabejacite is triclinic, space group P, with a = 8.7434(11), b = 8.309(3), c = 8.8693(10) Å , a = 77.86(2), b = 104.635(11), g = 82.935(18)°, V = 598.8(3) A˚ 3 and Z = 1, with Dcalc = 4.325 g cm–3. The structure refinement proved that rabejacite is related to the zippeite group of minerals, as it is based upon the structural sheets of the zippeite topology of composition [(UO2)4O4(SO4)2]4–. Located in the interlayer between the sheets, which are stacked perpendicular to [010], are Ca2+ cations and H2O groups. Ca2+ ions are [7]-coordinated, by three uranyl O atoms from adjacent sheets and four H2O groups. An additional H2O group, which is not bonded directly to any cation, is located in the interlayer. Along with rabejacite, its Cu-rich variety was found in the specimens examined and characterized structurally. Its crystal structure (R1 = 10.15% for 1049 reflections with I > 3s(I)) is practically the same as that of rabejacite, but there is an additional Cu2+ site located in between pairs of Ca polyhedra. The structural formula is (Ca1.56Cu0.40)Σ1.90[(UO2)4O4(SO4)2](H2O)8, Z = 1. Its existence suggests a greater diversity in zippeite crystal chemistry than was thought previously and also the possibility of a new Cu2+-dominant zippeite mineral besides pseudojohannite.
Švenekite, Ca[AsO2(OH)2]2, a new mineral from Jáchymov, Czech Republic
- P. Ondruš, R. Skála, J. Plášil, J. Sejkora, F. Veselovský, J. Čejka, A. Kallistová, J. Hloušek, K. Fejfarová, R. Škoda, M. Dušek, A. Gabašová, V. Machovič, L. Lapčák
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- Mineralogical Magazine / Volume 77 / Issue 6 / August 2013
- Published online by Cambridge University Press:
- 05 July 2018, pp. 2711-2724
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Švenekite (IMA 99-007), Ca[AsO2(OH)2]2, is a rare supergene arsenate mineral occurring in the Geschieber vein, Jáchymov ore district, Western Bohemia, Czech Republic. It grows directly on the granite rocks and occurs isolated from other arsenate minerals otherwise common in Jáchymov. Švenekite usually forms clear transparent coatings composed of indistinct radiating to rosette-shaped aggregates up to 3 mm across. They are composed of thin lens- or bladed-shaped crystals, usually 100 – 150 μm long. Švenekite is transparent to translucent and has a white streak and a vitreous lustre; it does not fluoresce under ultraviolet light. Cleavage is very good on {010}. The Mohs hardness is ∼2. Švenekite is biaxial, non-pleochroic. The refractive indices are α' = 1.602(2), γ' = 1.658(2). The empirical formula of švenekite (based on As + P + S = 2 a.p.f.u., an average of 10 spot analyses) is (Ca1.00Mg0.01)Σ1.01[AsO2(OH)2]1.96[PO2(OH)2]0.03(SO4)0.01. The simplified formula is Ca[AsO2(OH)2]2 and requires CaO 17.42, As2O571.39, H2O 11.19, total 100.00 wt.%. Raman and infrared spectroscopy exhibit dominance of O – H vibrations and vibration modes of distorted tetrahedral AsO2(OH)2 units. Švenekite is triclinic, space group P, with a = 8.5606(5), b = 7.6926(6), c = 5.7206(4) Å, α = 92.605(6), β = 109.9002(6), γ = 109.9017(6)º, and V = 327.48(4) Å3, Z = 2, Dcalc = 3.26 g·cm–3. The a:b:c ratio is 0.7436:1:1.1082 (for single-crystal data). The six strongest diffraction peaks in the X-ray powder diffraction pattern are [d (Å)/I(%)/(hkl)]: 3.968(33)(20); 3.766(35)(2); 3.697(49)(101); 3.554(100)(020); 3.259(33)(20); 3.097(49)(11). The crystal structure of švenekite was refined from single-crystal X-ray diffraction data to R1 = 0.0250 based on 1309 unique observed, and to wR2 = 0.0588, for all 1588 unique reflections (with GOFall = 1.20). The structure of švenekite consists of sheets of corner-sharing CaO8 polyhedra and AsO2 OH2 groups, stacked parallel to (001). Adjacent sheets are linked by hydrogen bonds. The švenekite structure possesses very short symmetrical hydrogen bonds (with the D–H lengths ∼1.22 Å). The mineral is named to honour Jaroslav Švenek, the former curator of the mineralogical collection of the National Museum in Prague, Czech Republic.
Hydroniumjarosite, (H3O)+Fe3(SO4)2(OH)6, from Cerros Pintados, Chile: Single-crystal X-ray diffraction and vibrational spectroscopic study
- J. Plášil, R. Škoda, K. Fejfarová, J. Čejka, A. V. Kasatkin, M. Dušek, D. Talla, L. Lapčák, V. Machovič, M. Dini
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- Mineralogical Magazine / Volume 78 / Issue 3 / June 2014
- Published online by Cambridge University Press:
- 05 July 2018, pp. 535-547
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The natural hydroniumjarosite sample from Cerros Pintados (Chile) was investigated by electron microprobe, single-crystal X-ray diffraction and vibrational spectroscopy (Infrared and Raman). The chemical composition of studied specimens (wt.%, mean of seven analyses) obtained from electron microprobe (in wt.%): Na2O 1.30, K2O 0.23, CaO 0.04, Fe2O3 50.49, Al2O3 0.37, SiO2 0.33, SO3 33.88, H2O (calculated on the basis of Σ(OH–+H3O+) deduced from the charge balance) 13.32, total 99.98, corresponds to the empirical formula (H3O)0.77+(Na0.20K0.02)∑0.22(Fe2.95Al0.03)∑2.98 (OH)6.12[(SO4)1.97(SiO4)0.03]∑2.00 (calculated on the basis of S + Si = 2 a.p.f.u. (atoms per formula unit)). The studied hydroniumjarosite is trigonal, with space group Rm, with a = 7.3408(2), c = 17.0451(6) Å and V = 795.46(4) Å3. The refined structure architecture is consistent with known jarosite-series minerals, including synthetic hydroniumjarosite. However, in the current study the presence of H3O+ is well documented in difference Fourier maps, where characteristic positive difference Fourier maxima, with apparent trigonal symmetry, were localized in the vicinity of the O4 atom in the channel-voids of the structure. The structure of natural hydroniumjarosite, including the H atoms, was refined to R1 = 0.0166 for 2113 unique observed reflections, with Iobs>3σ(I). The present structure model, which includes the position of the H atom within the hydronium ion, is discussed with regard to the vibration spectroscopy results and earlier published density-functional theory (DFT) calculations for the alunite-like structure containing H3O+.
Bêhounekite, U(SO4)2(H2O)4, from Jáchymov (St Joachimsthal), Czech Republic: the first natural U4+ sulphate
- J. Plášil, K. Fejfarová, M. Novák, M. Dušek, R. Škoda, J. Hloušek, J. Čejka, J. Majzlan, J. Sejkora, V. Machovic, D. Talla
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- Mineralogical Magazine / Volume 75 / Issue 6 / December 2011
- Published online by Cambridge University Press:
- 05 July 2018, pp. 2739-2753
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Bêhounekite, orthorhombic U(SO4)2(H2O)4, is the first natural sulphate of U4+. It was found in the Geschieber vein, Jáchymov (St Joachimsthal) ore district, Western Bohemia, Czech Republic, crystallized on the altered surface of arsenic and associated with kaatialaite, arsenolite, claudetite, unnamed phase UM1997-20-AsO:HU and gypsum. Bêhounekite most commonly forms short-prismatic to tabular green crystals, rarely up to 0.5 mm long. The crystals have a strong vitreous lustre and a grey to greenish grey streak. They are brittle with an uneven fracture and have very good cleavage along ﹛100﹜. The Mohs hardness is about 2. The mineral is not fluorescent either in short- or long-wavelength UV radiation. Bêhounekite is moderately pleochroic, α∼β is pale emerald green and γ is emerald green, and is optically biaxial (+) with α = 1.590(2), β = 1.618(4), γ = 1.659(2) (590 nm), 2V (calc.) = 81°, birefringence 0.069. The empirical formula of bêhounekite (based on 12 O atoms, from an average of five point analyses) is (U0.99Y0.03)Σ1.02(SO4)1.97(H2O)4. The simplified formula is U(SO4)2(H2O)4, which requires UO2 53.77. SO3 31.88, H2O 14.35, total 100.00 wt.%. Bêhounekite is orthorhombic, space group Pnma, a = 14.6464(3), b = 11.0786(3), c = 5.6910(14) Å, V = 923.43(4) Å3, Z = 4, Dcalc = 3.62 g cm–3. The seven strongest diffraction peaks in the X-ray powder diffraction pattern are [dobs in Å (I) (hid)]: 7.330 (100) (200), 6.112 (54) (210), 5.538 (21) (020), 4.787 (42) (111), 3.663 (17) (400), 3.478 (20) (410), 3.080 (41) (321). The crystal structure of bêhounekite has been solved by the charge-flipping method from single-crystal X-ray diffraction data and refined to R1 = 2.10 % with a GOF = 1.51, based on 912 unique observed diffractions. The crystal structure consists of layers built up from [8]-coordinate uranium atoms and sulphate tetrahedra. The eight ligands include four oxygen atoms from the sulphate groups and four oxygen atoms from the H2O molecules. Each uranium coordination polyhedron is connected via sulphate tetrahedra with other uranium polyhedra and through hydrogen bonds to the apices of sulphate tetrahedra. The dominant features of the Raman and infrared spectra of bêhounekite are related to stretching vibrations of SO4 tetrahedra (∼1200–950 cm–1), O-H stretching modes (∼3400–3000 cm–1) and H—O—H bending modes (∼1650 cm–1). The mineral is named in honour of František Bêhounek, a well known Czech nuclear physicist.
Leydetite, Fe(UO2)(SO4)2(H2O)11, a new uranyl sulfate mineral from Mas d’Alary, Lodève, France
- J. Plášil, A. V. Kasatkin, R. Škoda, M. Novák, A. Kallistová, M. Dušek, R. Skála, K. Fejfarová, J. Čejka, N. Meisser, H. Goethals, V. Machovič, L. Lapčák
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- Mineralogical Magazine / Volume 77 / Issue 4 / June 2013
- Published online by Cambridge University Press:
- 05 July 2018, pp. 429-441
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Leydetite, monoclinic Fe(UO2)(SO4)2(H2O)11(IMA 2012–065), is a new supergene uranyl sulfate from Mas d'Alary, Lodève, Hérault, France. It forms yellow to greenish, tabular, transparent to translucent crystals up to 2 mm in size. Crystals have a vitreous lustre. Leydetite has a perfect cleavage on (001). The streak is yellowish white. Mohs hardness is ∼2. The mineral does not fluoresce under long- or short-wavelength UV radiation. Leydetite is colourless in transmitted light, non-pleochroic, biaxial, with α = 1.513(2), γ = 1.522(2) (further optical properties could not be measured). The measured chemical composition of leydetite, FeO 9.28, MgO 0.37, Al2O30.26, CuO 0.14, UO340.19, SO321.91, SiO20.18, H2O 27.67, total 100 wt.%, leads to the empirical formula (based on 21 O a.p.f.u.), (Fe0.93Mg0.07Al0.04Cu0.01)Σ1.05(U1.01O2)(S1.96Si0.02)Σ1.98O8(H2O)11. Leydetite is monoclinic, space group C2/c, with a = 11.3203(3), b = 7.7293(2), c = 21.8145(8) Å, β = 102.402(3)°, V = 1864.18(10) Å3, Z = 4, and Dcalc = 2.55 g cm–3. The six strongest reflections in the X-ray powder diffraction pattern are [dobs in Å (I) (hkl)]: 10.625 (100) (002), 6.277 (1) (11), 5.321 (66) (004), 3.549 (5) (006), 2.663 (4) (008), 2.131 (2) (0 0 10). The crystal structure has been refined from single-crystal X-ray diffraction data to R1 = 0.0224 for 5211 observed reflections with [I > 3σ(I)]. Leydetite possesses a sheet structure based upon the protasite anion topology. The sheet consists of UO7 bipyramids, which share four of their equatorial vertices with SO4 tetrahedra. Each SO4 tetrahedron, in turn, shares two of its vertices with UO7 bipyramids. The remaining unshared equatorial vertex of the bipyramid is occupied by H2O, which extends hydrogen bonds within the sheet to one of a free vertex of the SO4 tetrahedron. Sheets are stacked perpendicular to the c direction. In the interlayer, Fe2+ ions and H2O groups link to the sheets on either side via a network of hydrogen bonds. Leydetite is isostructural with the synthetic compound Mg(UO2)(SO4)2(H2O)11. The name of the new mineral honours Jean Claude Leydet (born 1961), an amateur mineralogist from Brest (France), who discovered the new mineral.
Meisserite, Na5(UO2)(SO4)3(SO3OH)(H2O), a new uranyl sulfate mineral from the Blue Lizard mine, San Juan County, Utah, USA
- J. Plášil, A. R. Kampf, A. V. Kasatkin, J. Marty, R. Škoda, S. Silva, J. Čejka
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- Mineralogical Magazine / Volume 77 / Issue 7 / October 2013
- Published online by Cambridge University Press:
- 05 July 2018, pp. 2975-2988
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Meisserite (IMA2013-039), Na5(UO2)(SO4)3(SO3OH)(H2O), is a new uranyl sulfate mineral from the Blue Lizard mine, San Juan County, Utah (USA). It is named in honour of the prominent Swiss mineralogist Nicolas Meisser. The new mineral was found in a sandstone matrix and is associated with chalcanthite, copiapite, ferrinatrite, gypsum, johannite and another new Na-bearing uranyl sulfate, belakovskiite (IMA2013-075). Meisserite is a secondary mineral formed by the post-mining weathering of uraninite. The mineral is triclinic, P, a = 5.32317(10), b = 11.5105(2), c = 13.5562(10) Å, α = 102.864(7)°, β = 97.414(7)°, γ = 91.461(6)°, V = 801.74(6) Å3, and Z = 2. Crystals are prisms elongated on [100], up to 0.3 mm long, exhibiting the forms {010} and {001}. Meisserite is pale green to yellowish green, translucent to transparent and has a very pale yellow streak. It is brittle, with fair cleavage on {100} and {001}, and uneven fracture. The Mohs hardness is estimated at 2. Meisserite is somewhat hygroscopic and easily soluble in water. The calculated density based on the empirical formula is 3.208 g/cm3. Meisserite exhibits bright yellow green fluorescence under both long- and shortwave UV radiation. The mineral is optically biaxial (–), with α = 1.514(1), β = 1.546(1), γ = 1.557(1) (measured in white light). The measured 2V is 60(2)° and the calculated 2V is 60°. Dispersion is r > v, perceptible, and the optical orientation is X ≈ a, Z ≈ c*. The mineral is pleochroic, with X (colourless) < Y (pale yellow) ≈ Z (pale greenish yellow). The empirical formula of meisserite (based on 19 O a.p.f.u.) is Na5.05(U0.94O2)(SO4)3[SO2.69(OH)1.31](H2O). The Raman spectrum is dominated by the symmetric stretching vibrations of UO22+, SO42– and also weaker O–H stretching vibrations. The eight strongest powder X-ray diffraction lines are [dobs in Å (hkl)Irel]: 13.15 (001) 81, 6.33 (02) 62, 5.64 (01,020) 52, 5.24 (100,012,01) 100, 4.67 (101) 68, 3.849 (1,102,022) 48, 3.614 (02,3) 41, and 3.293 (13,004) 43. The crystal structure of meisserite (R1 = 0.018 for 3306 reflections with Iobs > 3σI) is topologically unique among known structures of uranyl minerals and inorganic compounds. It contains uranyl pentagonal bipyramids linked by SO4 groups to form chains. Na+ cations bond to O atoms in the chains and to an SO3OH group and an H2>O group between the chains, thereby forming a heteropolyhedral framework.
The crystal chemistry of the uranyl carbonate mineral grimselite, (K, Na)3Na[(UO2)(CO3)3](H2O), from Jáchymov, Czech Republic
- J. Plášil, K. Fejfarová, R. Skála, R. Škoda, N. Meisser, J. Hlousek, I. Císařová, M. Dušek, F. Veselovský, J. Čejka, J. Sejkora, P. Ondruš
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- Mineralogical Magazine / Volume 76 / Issue 3 / June 2012
- Published online by Cambridge University Press:
- 05 July 2018, pp. 443-453
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Two crystals of the uranyl carbonate mineral grimselite, ideally K3Na[(UO2)(CO3)3](H2O), from Jáchymov in the Czech Republic were studied by single-crystal X-ray diffraction and electron-probe microanalysis. One crystal has considerably more Na than the ideal chemical composition due to substitution of Na into KO8 polyhedra; the composition of the other crystal is nearer to ideal, and similar to synthetic grimselite. The presence of Na atoms in KO8 polyhedra, which are located in channels in the crystal structure, reduces their volume, and as a result the unit-cell volume also decreases. Structure refinement shows that the formula for the sample with the anomalously high Na content is (K2.43Na0.57)Σ3.00Na[(UO2)(CO3)3](H2O). The unit-cell parameters, refined in space group P2c, are a = 9.2507(1), c = 8.1788(1) Å, V = 606.14(3) Å3 and Z = 2. The crystal structure was refined to R1 = 0.0082 and wR1 = 0.0185 with a GOF = 1.33, based on 626 observed diffraction peaks [Iobs>3σ(I)].
An XRD, SEM and TG study of a uranopilite from Australia
- R.L. Frost, M.L. Weier, G.A. Ayoko, W. Martens, J. Čejka
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- Mineralogical Magazine / Volume 70 / Issue 3 / June 2006
- Published online by Cambridge University Press:
- 05 July 2018, pp. 299-307
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A uranopilite from The South Alligator River, Northern Territory, Australia, has been studied using X-ray diffraction (XRD), scanning electron microscopy (SEM) with EDAX attachment, and thermogravimetry in conjunction with evolved gas mass spectrometry. The XRD shows that the mineral is a pure uranopilite with few if any impurities. The SEM images show that the uranopilite consists of elongated crystals, up to 50μm long and 5 μm wide. Thermogravimetry combined with mass spectrometry shows that dehydration occurs at ∼31°C resulting in the formation of metauranopilite. The first dehydration step over 20–71°C corresponds to a decrease of 5.4 wt.%, equivalent to 6.076 H2O. The second dehydration step, over the temperature range 71 –162.4°C corresponds to a decrease of 4.7 wt.%, equivalent to 5.288 H2O, making a total of 11.364 moles of H2O, close to 12 H2O for uranopilite.
Dehydroxylation takes place over the temperature range 80–160°C. The loss of sulphate occurs at higher temperatures in two steps at 622 and 636°C. A mass loss also occurs at 755°C, accounted for by evolved oxygen.
Vysokýite, U4+[AsO2(OH)2]4·4H2O, a new mineral from Jáchymov, Czech Republic
- J. Plášil, J. Hloušek, R. Škoda, M. Novák, J. Sejkora, J. Čejka, F. Veselovský, J. Majzlan
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- Mineralogical Magazine / Volume 77 / Issue 8 / December 2013
- Published online by Cambridge University Press:
- 05 July 2018, pp. 3055-3066
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Vysokýite, U4+[(AsO2(OH)2]4(H2O)4 (IMA 2012–067), was found growing on an altered surface of massive native As in the Geschieber vein, Jáchymov ore district, Western Bohemia, Czech Republic. The new mineral was found in association with běhounekite, štěpite, kaatialaite, arsenolite, claudetite and gypsum. It forms extremely fibrous light-green crystals up to 8 mm long. Crystals have an alabaster lustre and a greenish-white to greyish streak. Vysokýite is brittle with uneven fracture and perfect cleavage along (100) and (001); the Mohs hardness is ∼2. A density of 3.393 g/cm3 was calculated using the empirical formula and unit-cell parameters obtained from a single-crystal diffraction experiment. Vysokýite is non-fluorescent under short or long wavelength UV radiation. It is colourless under the microscope, measured refractive indices are α' = 1.617(3), γ' = 1.654(3); the estimated optical orientation is α' ∼X, γ' ∼Z. The average of five spot wavelength dispersive spectroscopy (WDS) analyses is 29.44 UO2, 1.03 SiO2, 48.95 As2O5, 0.12 SO3, 15.88 H2O (calc.), total 95.42 wt.%. The empirical formula of vysokýite (based on 20 O a.p.f.u.) is U1.00[AsO2(OH)2]3.90(SiO4)0.16 (SO4)0.01·4H2O. The As–O–H and O–H vibrations dominate in the Raman spectrum. Vysokýite is triclinic, space group P, with a = 10.749(2), b = 5.044(3), c = 19.1778(7) Å, α = 89.872(15)°, β = 121.534(15)°, γ = 76.508(15)°, and V = 852.1(6) Å3, Z = 2 and Dcalc = 3.34 g·cm–3. The strongest diffraction peaks in the X-ray powder diffraction pattern are [dobs in Å (Irel.)(hkl)]: 8.872(100)(100), 8.067(50)(002), 6.399(7)(10), 4.773(6)(10), 3.411(10)(30), 3.197(18)(31). The crystal structure of vysokýite was solved from single-crystal X-ray diffraction data by the charge-flipping method and refined to R1 = 0.0595 based on 2718 unique observed reflection, and to wR2 = 0.1160 for all 4173 unique reflections. The structure of vysokýite consists of UO8 square antiprisms sharing all of their vertices with 8 As-tetrahedra to form infinite chains parallel to [010]. These chains are linked by hydrogen bonds involving terminal (OH) groups of the double-protonated As-tetrahedra and molecules of H2O located between the chains. The new mineral is named in honour of Arnošt Vysoký (1823–1872), the former chief of the Jáchymov mines and smelters, chemist and metallurgist.
Tvrdýite, Fe2+Fe32+Al3(PO4)4(OH)5(OH2)4·2H2O, a new phosphate mineral from Krásno near Horní Slavkov, Czech Republic
- J. Sejkora, I. E. Grey, A. R. Kampf, J. R. Price, J. Čejka
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- Journal:
- Mineralogical Magazine / Volume 80 / Issue 6 / October 2016
- Published online by Cambridge University Press:
- 02 January 2018, pp. 1077-1088
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Tvrdýite, Fe2+Fe3+2A13(PO4)4(OH)5(OH2)4·2H2O, is a new phosphate mineral from the abandoned Huber open pit, in the Krásno ore district near Horní Slavkov, western Bohemia, Czech Republic. It was found along with Al-rich beraunite, fluorapatite and pharmacosiderite in a cavity of quartz gangue. Tvrdýite forms acicular to fibrous crystals with diameters in the range 0.5–5 μm and lengths up to 300 μm, partly grouped in radiating aggregates up to 3 mm in size. It has a silvery to olive, greyish green colour with pearly lustre, greyish-white streak and is very brittle with an uneven fracture; individual fibres are somewhat flexible. Cleavage on {100} is good; the Mohs hardness is ∼3–4. The calculated density is 2.834 g cm–3. Tvrdýite is optically biaxial (–), with α = 1.650(2), β = 1.671(1) and γ = 1.677(1) (white light); 2V = 56(1)°; dispersion: r > v, strong; optical orientation: Z = b, X ≈ a, Y ≈ c; pleochroism: X = greenish blue, Y = yellowish orange, Z = yellowish orange (X>> Y > Z). Tvrdýite is monoclinic, space group C2/c, a = 20.564(4), b = 5.101(1), c = 18.883(4) Å, β = 93.68(3)° and V = 1976.7(7) Å3, Z = 4, a:b:c= 4.031:1:3.702. The strongest eight lines in the powder X-ray diffraction (XRD) pattern [d in Å (I)(hkl)] are 10.227 (100) (200), 9.400 (6) (002), 7.156 (14) (202), 5.120 (7) (400), 3.416 (11) (600), 3.278 (6) (602), 2.562 (5) (800) and 2.0511 (3) (10,0,0). Chemical analyses by electron microprobe yielded MnO 0.01, ZnO 5.08, , FeO 4.31, Fe2O3 21.16, Al2O316.71, P2O5 32.64, As2O5 2.56, F 0.53, H2O (calc.) 17.84, O = F –0.22, total 100.62 wt.%. The resulting empirical formula, calculated on the base of 27 anions, obtained from the crystal structure, is Zn0.52Fe2+0.50Fe3+2.21Al2.75(PO4)3.86(AsO4)0.19OH4.60F0.23(OH2)4·2H2O. The ideal formula, Fe2+Fe3+2Al3(PO4)4(OH)5(OH2)4-2H2O, requires FeO 8.75, Fe2O3 19.44, Al2O3 18.62, P2O5 34.56, H2O 18.64, total 100.00 wt.%. The crystal structure of tvrdýite was solved from single-crystal data (synchrotron beamline) and refined to R1 = 0.038 for 2276 reflections with I > 2σ(I). Tvrdýite is isostructural with beraunite, but contains dominant Al in two of the four independent M sites, which are all occupied by Fe in beraunite.
Geschieberite, K2(UO2)(SO4)2(H2O)2, a new uranyl sulfate mineral from Jáchymov
- J. Plášil, J. Hloušek, A. V. Kasatkin, R. Škoda, M. Novák, J. Čejka
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- Journal:
- Mineralogical Magazine / Volume 79 / Issue 1 / February 2015
- Published online by Cambridge University Press:
- 02 January 2018, pp. 205-216
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The new mineral geschieberite (IMA2014-006), K2(UO2)(SO4)2(H2O)2, was found in the Svornost mine, Jáchymov, Czech Republic, where it occurs as a secondary alteration phase after uraninite in association with adolfpateraite and gypsum. Geschieberite forms crystalline aggregates of bright green colour (when thick) composed of multiply intergrown prismatic crystals elongated on [001] typically reaching 0.1–0.2 mm across; observable forms are {010} and {001}. Crystals are translucent to transparent with a vitreous lustre. The mineral is brittle, with perfect cleavage on {100} and an uneven fracture. It has a greenish-white streak and a probable Mohs hardness of ∼2. The mineral is slightly soluble in cold H2O. The calculated density is 3.259 g cm–3. The mineral exhibits strong yellowish-green fluorescence under both shortwave and longwave UV radiation. Optically, geschieberite is biaxial (–), with β = 1.596(2) and γ = 1.634(4) (measured at 590 nm), with X = a. Electron-microprobe analyses provided Na2O 0.23, K2O 14.29, MgO 2.05, CaO 0.06, UO3 49.51, SO3 27.74, H2O 6.36 (structure), total 100.24 wt.%, yielding the empirical formula (K1.72Mg0.29Na0.04Ca0.01)Σ2.06(U0.98O2)(S0.98O4)2(H2O)2 based on 12 O atoms per formula unit. The Raman spectrum is dominated by the symmetric stretching vibrations of UO22+, SO42– and weaker O–H stretching vibrations. Geschieberite is orthorhombic, Pna21, with a = 13.7778(3), b = 7.2709(4), c = 11.5488(2) Å, V = 1156.92(7) Å3, Z = 4. The eight strongest powder X-ray diffraction lines are [dobs in Å (hkl) Irel]: 6.882 (200) 100, 5.622 (111) 53, 4.589 (211) 12, 4.428 (202) 16, 3.681 (311) 18, 3.403 (013) 12, 3.304 (401,1̄13) 15 and 3.006 (122) 17. The structure, refined to R = 0.028 for 1882 I > 3σ(I) reflections, contains [(UO2)(SO4)2(H2O)]2– sheets that are based on the protasite anion topology. Sheets are stacked perpendicular to a. Potassium atoms and one H2O molecule are located between these sheets, providing an interlayer linkage. The remaining H2O molecule is localized within the structural unit, at the free vertex of the uranyl pentagonal bipyramid; this vertex does not link to sulfate tetrahedra. The mineral is named for one of the most important ore veins in Jáchymov – the Geschieber vein.