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1.
  • Biagion, Cristian, et al. (författare)
  • The crystal structure of turneaureite, Ca5(AsO4)3Cl, the arsenate analog of chlorapatite and its relationships with the arsenate apatites johnbaumite and svabite
  • 2017
  • Ingår i: American Mineralogist. - 0003-004X. ; 102, s. 1981-1986
  • Tidskriftsartikel (refereegranskat)abstract
    • The crystal structure of turneaureite, ideally Ca5(AsO4)3Cl, was studied using a specimen from the Brattfors mine, Nordmark, Värmland, Sweden, by means of single-crystal X-ray diffraction data. The structure was refinedto R1 = 0.017 on the basis of 716 unique reflectios with Fo > 4σ(Fo) in the P63/m space group, with unit-cell parameters a = 9.9218(3), c = 6.8638(2) Å, V = 585.16(4) Å3. The chemical composition of the sample, determined by electron-microprobe analysis, is (in wt%; average of 10 spot analyses): SO3 0.22, P2O5 0.20, V2O5 0.01, As2O5 51.76, SiO2 0.06, CaO 41.39, MnO 1.89, SrO 0.12, BaO 0.52, PbO 0.10, Na2O 0.02, F 0.32, Cl 2.56, H2Ocalc 0.58, O(≡F+Cl) –0.71, total 99.04. On the basis of 13 anions per formula unit, the empirical formula corresponds to (Ca4.82Mn0.17Ba0.02Sr0.01)∑5.02 (As2.94P0.02S0.02Si0.01)∑2.99O12[Cl0.47(OH)0.42F0.11]∑1.00.Turneaureite is topologically similar to the other members of the apatite supergroup: columns of face-sharing M1 polyhedra running along c are connected through TO4 tetrahedra with channels hosting M2 cations and X anions. Owing to its particular chemical composition, the studied turneaureite can be considered as a ternary calcium arsenate apatite; consequently it has several partially filledanion sites within the anion columns. Polarized single-crystal FTIR spectra of the studied sample indicate stronger hydrogen bonding and less diverse short-range atom arrangements around (OH) groups in turneaureite as compared to the related minerals johnbaumite and svabite. An accurate knowledge of the atomic arrangement of this apatite-remediation mineral represents an improvement in our understanding of minerals able to sequester and stabilize heavy metals such as arsenic in polluted areas.
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  • Nilsson, E.J. Charlotta, et al. (författare)
  • A nuclear geochemical analysis system for boron quantification using a focused ion beam
  • 2017
  • Ingår i: Journal of Radioanalytical and Nuclear Chemistry. - Kluwer. - 0236-5731. ; 311:1, s. 355-364
  • Tidskriftsartikel (refereegranskat)abstract
    • Ion beam analysis has for decades been used as a tool for geochemical analysis of trace elements using both X-rays (particle induced X-ray emission) and nuclear reaction analysis. With the geoanalytical setup at the Lund Ion Beam Analysis Facility, the boron content in geological samples with a spatial resolution of 1 µm is determined through nuclear reaction analysis. In the newly upgraded setup, a single detector has been replaced by a double sided silicon strip detector with 2048 segments. After optimization, boron content in geological samples as low as 1 µg g−1 can be measured.
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  • Biagioni, Cristian, et al. (författare)
  • The crystal structure of svabite, Ca5(AsO4)3F, an arsenate member of the apatite supergroup
  • 2016
  • Ingår i: American Mineralogist. - 0003-004X. ; 101, s. 1750-1755
  • Tidskriftsartikel (refereegranskat)abstract
    • The crystal structure of svabite, ideally Ca5(AsO4)3F, was studied using a specimen from the Jakobsberg mine, Värmland, Sweden, by means of single-crystal X‑ray diffraction data. The structure was refined to R1 = 0.032 on the basis of 928 unique reflections with Fo > 4s(Fo) in the P63/m space group, with unit-cell parameters a = 9.7268(5), c = 6.9820(4) Å, V = 572.07(5) Å3. The chemical composition of the sample, determined by electron-microprobe analysis, is (in wt%, average of 10 spot analyses): SO3 0.49, P2O5 0.21, V2O5 0.04, As2O5 51.21, SiO2 0.19, CaO 39.31, MnO 0.48, SrO 0.03, PbO 5.19, Na2O 0.13, F 2.12, Cl 0.08, H2Ocalc 0.33, O (≡ F+Cl) –0.91, total 98.90. On the basis of 13 anions per formula unit, the empirical formula corresponds to (Ca4.66Pb0.16Mn0.04Na0.03)Σ4.89(As2.96S0.04Si0.02P0.02)Σ3.04O12[F0.74(OH)0.24Cl0.01]. Svabite is topologically similar to the other members of the apatite supergroup: columns of face-sharing M1 polyhedra running along c are connected through TO4 tetrahedra with channels hosting M2 cations and X anions. The crystal structure of synthetic Ca5(AsO4)3F was previously reported as triclinic. On the contrary, the present refinement of the crystal structure of svabite shows no deviations from the hexagonal symmetry. An accurate knowledge of the atomic arrangement of this apatite-remediation mineral represents an improvement in our understanding of minerals able to sequester and stabilize heavy metals such as arsenic in polluted areas.
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  • Bosi, Ferdinando, et al. (författare)
  • Crystal chemistry of spinels in the system MgAl2O4-MgV2O4-Mg2VO4
  • 2016
  • Ingår i: American Mineralogist. - 0003-004X. ; 101, s. 580-586
  • Tidskriftsartikel (refereegranskat)abstract
    • Eight spinel single-crystal samples belonging to the spinel sensu stricto-magnesiocoulsonite series (MgAl2O4-MgV2O4) were synthesized and crystal-chemically characterized by X‑ray diffraction, electron microprobe and optical absorption spectroscopy. Site populations show that the tetrahedrally coordinated site (T) is populated by Mg and minor Al for the spinel sensu stricto compositions, and only by Mg for the magnesiocoulsonite compositions, while the octahedrally coordinated site (M) is populated by Al, V3+, minor Mg, and very minor amounts of V4+. The latter occurs in appreciable amounts in the Al-free magnesium vanadate spinel, T(Mg)M(Mg0.26V3+1.48V4+0.26)O4, showing the presence of the inverse spinel VMg2O4. The studied samples are characterized by substitution of Al3+ for V3+ and (Mg2++V4+) for 2V3+ described in the system MgAl2O4-MgV2O4-VMg2O4.The present data in conjunction with data from the literature provide a basis for quantitative analyses of two solid-solution series MgAl2O4-MgV23+O4 and MgV23+O4-V4+Mg2O4. Unit-cell parameter increases with increasing V3+ along the series MgAl2O4-MgV2O4 (8.085–8.432 Å), but only slightly increases with increasing V3+ along the series VMg2O4-MgV2O4 (8.386–8.432 Å). Although a solid solution could be expected between the MgAl2O4 and VMg2O4 end-members, no evidence was found. Amounts of V4+ are nearly insignificant in all synthetic Al-bearing vanadate spinels, but are appreciable in Al-free vanadate spinel.An interesting observation of the present study is that despite the observed complete solid-solution along the MgAl2O4-MgV2O4 and MgV2O4-VMg2O4 series, the spinel structure seems to be unable to stabilize V4+ in any intermediate members on the MgAl2O4-Mg2VO4 join even at high oxygen fugacities. This behavior indicates that the accommodation of specific V-valences can be strongly influenced by crystal-structural constraints, and any evaluation of oxygen fugacities during mineral formation based exclusively on V cation valence distributions in spinel should be treated with caution. The present study underlines that the V valency distribution in spinels is not exclusively reflecting oxygen fugacities, but also depends on activities and solubilities of all chemical components in the crystallization environment.
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15.
  • Bosi, Ferdinando, et al. (författare)
  • Thermally induced cation redistribution in Fe‑bearing oxy‑dravite and potential geothermometric implications
  • 2016
  • Ingår i: Contributions to Mineralogy and Petrology. - 0010-7999. ; 171:5, s. 1-14
  • Tidskriftsartikel (refereegranskat)abstract
    • Iron-bearing oxy-dravite was thermally treated in air and hydrogen atmosphere at 800 °C to study potential changes in Fe, Mg and Al ordering over the octahedrally coordinated Y and Z sites and to explore possible applications to intersite geothermometry based on tourmaline. Overall, the experimental data (structural refinement, Mössbauer, infrared and optical absorption spectroscopy) show that heating Fe-bearing tourmalines results in disordering of Fe over Y and Z balanced by ordering of Mg at Y, whereas Al does not change appreciably. The Fe disorder depends on temperature, but less on redox conditions. The degree of Fe3+–Fe2+ reduction is limited despite strongly reducing conditions, indicating that the fO2 conditions do not exclusively control the Fe oxidation state at the present experimental conditions. Untreated and treated samples have similar short- and long-range crystal structures, which are explained by stable Al-extended clusters around the O1 and O3 sites. In contrast to the stable Al clusters that preclude any temperature-dependent Mg–Al order– disorder, there occurs Mg diffusion linked to temperaturedependent exchange with Fe. Ferric iron mainly resides around O2− at O1 rather than (OH)−, but its intersite disorder induced by thermal treatment indicates that Fe redistribution is the driving force for Mg–Fe exchange and that its diffusion rates are significant at these temperatures. With increasing temperature, Fe progressively disorders over Y and Z, whereas Mg orders at Y according to the order–disorder reaction: YFe + ZMg → ZFe + YMg. The presented findings are important for interpretation of the post-crystallization history of both tourmaline and tourmaline host rocks and imply that successful tourmaline geothermometers may be developed by thermal calibration of the Mg– Fe order–disorder reaction, whereas any thermometers based on Mg–Al disorder will be insensitive and involve large uncertainties.
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16.
  • Deegan, F.M., et al. (författare)
  • Pyroxene standards for SIMS oxygen isotope analysis and their application to Merapi volcano, Sunda arc, Indonesia
  • 2016
  • Ingår i: Chemical Geology. - 0009-2541. ; 447, s. 1-10
  • Tidskriftsartikel (refereegranskat)abstract
    • Measurement of oxygen isotope ratios in common silicate minerals such as olivine, pyroxene, feldspar, garnet, and quartz is increasingly performed by Secondary Ion Mass Spectrometry (SIMS). However, certain mineral groups exhibit solid solution series, and the large compositional spectrum of these mineral phases will result in matrix effects during SIMS analysis. These matrix effects must be corrected through repeated analysis of compositionally similar standards to ensure accurate results. In order to widen the current applicability of SIMS to solid solution mineral groups in common igneous rocks, we performed SIMS homogeneity tests on new augite (NRM-AG-1) and enstatite (NRM-EN-2) reference materials sourced from Stromboli, Italy and Webster, North Carolina, respectively. Aliquots of the standard minerals were analysed by laser fluorination (LF) to establish their δ18O values. Repeated SIMS measurements were then performed on randomly oriented fragments of the same pyroxene crystals, which yielded a range in δ18O less than ± 0.42 and ± 0.58‰ (2σ) for NRM-AG-1 and NRM-EN-2, respectively. Homogeneity tests verified that NRM-AG-1 and NRM-EN-2 do not show any crystallographic orientation bias and that they are sufficiently homogeneous on the 20 μm scale to be used as routine mineral standards for SIMS δ18O analysis. We subsequently tested our new standard materials on recently erupted pyroxene crystals from Merapi volcano, Indonesia. The δ18O values for Merapi pyroxene obtained by SIMS (n = 204) agree within error with the LF-derived δ18O values for Merapi pyroxene but differ from bulk mineral and whole-rock data obtained by conventional fluorination. The bulk samples are offset to higher δ18O values as a result of incorporation of mineral and glass inclusions that in part reflects crustal contamination processes. The Merapi pyroxene SIMS data, in turn, display a frequency peak at 5.8‰, which allows us to estimate the δ18O value of the primary mafic magma at Merapi to ~ 6.1‰ when assuming closed system differentiation.
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17.
  • Gatta, Diego, et al. (författare)
  • H-bonding scheme in allactite: a combined single-crystal X-ray and neutron diffraction, optical absorption spectroscopy, FTIR and EPMA-WDS study
  • 2016
  • Ingår i: Mineralogical magazine. - 0026-461X. ; 80:5, s. 719-732
  • Tidskriftsartikel (refereegranskat)abstract
    • The crystal chemistry of allactite from Långban, Värmland (Sweden) was investigated by single-crystal X-ray and neutron diffraction, optical absorption spectroscopy, Fourier-transform infra-red spectroscopy (FTIR) and electron microprobe analysis by wavelength-dispersive spectroscopy (EPMA-WDS). The optical spectra indicate the presence of Mn in valence state 2+ only. Assuming 16 O atoms per formula unit, arsenic as As5+ and the (OH) content calculated by charge balance, the resulting formula based on the EPMA-WDS data is (Mn6.732+Ca0.13Mg0.12Zn0.02)Σ7.00(As5+)2.00O16H8, very close to the ideal composition Mn7(AsO4)2(OH)8. In the unpolarized FTIR spectrum of allactite, fundamental (OH)-stretching bands are observed at 3236, 3288, 3387, 3446, 3484, 3562 and 3570 cm–1, suggesting that a number of OH environments, with different hydrogen bond strengths, occur in the structure. The neutron structure refinement shows that four independent H sites occur in allactite with full site occupancy, all as members of hydroxyl groups. The complex hydrogen-bonding scheme in the allactite structure is now well defined, with at least nine hydrogen bonds energetically favourable with mono-, bi- and trifurcated configurations.
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24.
  • Lenaz, Davide, et al. (författare)
  • Structural parameters of Cr-bearing spinels and pleonaste from the Cuillin Igneous Complex (Isle of Skye, Scotland): Implications for metamorphic and cooling history
  • 2016
  • Ingår i: Mineralogical magazine. - 0026-461X. ; 80:5, s. 749-764
  • Tidskriftsartikel (refereegranskat)abstract
    • The Outer Layered Suite of the Cuillin Igneous Complex (Isle of Skye, NW Scotland) comprises a Peridotite Series and a younger Allivalite Series (the latter comprising troctolites, eucrites and gabbros). Close to the junction between the Peridotite and the Allivalite Series (but wholly contained within the latter), an ultramafic breccia unit containing abundant peridotite xenoliths crops out. In the Peridotite Series, reddish-brown Cr-bearing spinels are present as disseminated crystals in the peridotite and also as chromitite seams, while in the peridotite xenoliths of the breccia unit, green pleonaste occurs in both of these modes of textural occurrence. Optical absorption spectroscopy reveals that the colour difference between the two spinel phases is related mainly to variable Al, Cr and Fe contents, while crystal structural analysis shows that the cooling rate calculated utilizing the oxygen positional parameter is comparable for all samples. The intracrystalline closure temperature for the Cr-spinel in the Peridotite Series is different for the disseminated and seam textural occurrences of the spinels, while the temperatures yielded by pleonaste in the peridotite xenoliths are the same for both textural occurrences. Our dataset suggests that the pleonaste in the peridotite xenoliths has been heated and equilibrated under subsolidus conditions, probably during breccia formation. During this heating, homogenization of the closure temperatures of pleonaste spinels occurred.
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