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Synthesis, crystal structure and magnetic properties of a new hydroxylammonium fluoroferrate
Brina Dojer, Matjaž Kristl, Zvonko Jagličić, Amalija Golobič, Marta Kasunič, Mihael Drofenik, 2012, original scientific article

Abstract: This paper reports on the synthesis of a new hydroxylammonium fluoroferrate, with the formula $(NH_3OH)_3FeF_6$, obtained after dissolving iron powder in hydrofluoric acid and adding solid $NH_3OHF$. This new compound has been characterized by chemical and thermal analysis, single-crystal X-ray diffraction, and magnetic measurements. The title compound crystallizes trigonal, R3c, with cell parameters a = 11.4154(2) Å, c = 11.5720(2) Å, Z = 6. The structure consists of $NH_3OH^+$ cations and isolated $FeF_6^{3–}$ octahedra in which the central ion lies on a threefold axis. The oxygen and nitrogen atoms of the hydroxylammonium cations are donors of hydrogen bonds to fluoride anions, resulting in a network of hydrogen bonds between counterions. The effective magnetic moment $µ_{eff}$ = 5.8 BM was calculated and perfectly matches the expected value of high-spin Fe(III) ions. The thermal decomposition of the compound was studied by TG, DSC, and X-ray powder diffraction.
Keywords: inorganic chemistry, crystallography, coordination compounds, synthesis, crystal structure, characterization of compounds, determination of the structure of compounds, X-ray diffraction, magnetic measurements, thermal analysis, TG, DSC, hydrogen bond, metal complexes, hydroxylammonium fluoromethalatehydroxylammonium, fluoroferrate
Published: 25.08.2017; Views: 1140; Downloads: 50
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Synthesis and characterisation of hydroxylammonium fluorochromate
Matjaž Kristl, Mihael Drofenik, Ljubo Golič, Amalija Golobič, 2003, original scientific article

Abstract: Reactions in the system $Cr – NH_3OHF – HF – H_2O$ were investigated. Green crystals of a new compound with the formula $(NH_3OH)_3CrF_6$ have been isolated from the water solution and characterized by chemical analysis. The compound crystallizes as triclinic, P-1, with cell parameters: a = 6.5461(2) Å, b = 6.9347(2) Å, c = 9.4072(3) Å, α = 86.772(1)°, β = 83.804(1)°, γ = 70.283(1)°. The effective magnetic moment, $µ_{eff}$ = 3.82 BM, was calculated from magnetic susceptibility measurements in the temperature range 80-290 K. The thermal decomposition of the compound was studied by TG and DSC analysis. $(NH_3OH)_3CrF_6$ decomposes above 125 °C in three steps and the residue has been identified by X-ray powder diffraction as $α – Cr_2O_3$.
Keywords: inorganic chemistry, structural chemistry, crystalline structure, coordination compounds, synthesis, inorganic reactions, thermal decomposition, characterization of compounds, TG, DSC, X-ray diffraction, chromium complexes, hydroxylammonium fluoro chromates, crystals
Published: 25.08.2017; Views: 949; Downloads: 81
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Ammoniumbis(hydroxylammonium) pentafluoridooxidovanadate(IV)
Brina Dojer, Matjaž Kristl, Zvonko Jagličić, Mihael Drofenik, Anton Meden, 2008, original scientific article

Abstract: Turquoise crystals of a new hydroxylammonium compound with the formula $NH_4(NH_3OH)_2[VOF_5]$ have been synthesized by the reaction of solid $NH_3OHF$ and the aqueous solution of vanadium in HF. The compound crystallizes monoclinic, $P2_1/n$, with cell parameters: a = 10.5658(2) Å, b = 6.6143(1) Å, c = 11.6618(2) Å, β = 96.282(1). Magnetic susceptibility was measured using a SQUID device over a temperature range 2–300 K at magnetic field $10^3 Oe$ giving the result $µ_{eff}$ = 1.65 BM. The thermal decomposition was studied by TG and DSC analysis. $NH_4(NH_3OH)_2[OF_5V]$ decomposes above 354 K in three steps, obtaining $NH_4VOF_3$ after the first step and $V_2O_5$ as the final residue.
Keywords: hydroxylammonium fluorovanadates, x-ray powder diffraction, x-ray structure determination, thermal analysis
Published: 17.08.2017; Views: 858; Downloads: 67
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Measurement of strain caused by residual stresses in a welded joint using neutron diffraction
Nenad Gubeljak, Jelena Vojvodič-Tuma, Hans-Georg Preismeyer, 1999, original scientific article

Abstract: The distribution and amount of residual stresses can significantly contrubute to the fatigue fracture behaviour of welded joints in structures. Interior residual stresses, which interact with the plane strain state, are more dangerous than residual stresses at the surface of the welded joint. If the surface of the welded joint is mechanically treated (e.g. shapering), then significant differences between the stress stated at the surface and within the volume occur. Hence, different non-destructive methods (e.g. gamma radiation, neutron diffraction) have been developed to determine strains caused by residual stresses in the volume of polycrystalline materials. However, the measurement of strains caused by residual stresses becomes difficult for large samples. In this paper the measurement procedure on a sample taken from the weld joint is presented and the effecet of residual stresses on fatigue crack propagation is assessed for low and high cycle loading fatigue.
Keywords: zaostale napetosti, zvarni spoj, neutronski lom žarkov, utrujenostno širjenje razpoke, neutron diffraction method, residual stresses, fatigue crack propagation, weld joint
Published: 10.07.2015; Views: 695; Downloads: 17
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Hydroxylammonium fluorogermanates
Irena Ban, Matjaž Kristl, Mihael Drofenik, Arkadije Popović, 2004, original scientific article

Abstract: A new hydroxylammonium compound (NH3OH)2GeF6, has been synthesized by the addition of solid NH3OHF to a solution of GeO2 dissolved in 20% HF. The compound was characterized by chemical analysis and X-ray powder diffraction, the thermal decomposition was studied by thermal analysis and mass spectrometry. (NH3OH)2GeF6 crystallizes monoclinic. Two endothermic and two exothermic peaks have been observed on the DSC curve, the decomposition product at 500 °C is GeO2.
Keywords: inorganic chemistry, synthesis, characterisation, hydroxylammonium fluorogermanates, x-ray powder diffraction, mass spectroscopy, thermal analysis
Published: 01.06.2012; Views: 1857; Downloads: 79
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Crystal-structure and Mössbauer studies of Li[sub]1.746]Nd[sub]4.494FeO9[sub]9.493
Mihael Drofenik, Irena Ban, Darko Makovec, Darko Hanžel, Amalija Golobič, Ljubo Golič, 2007, original scientific article

Abstract: The ▫$Li_1.746Nd_4.494FeO_9.493$▫ (LNF) ternary phase, located in the ▫$Li_2O$▫-rich part of the ▫$Li_2O-Nd_2O_3-Fe_2O_3$▫ system, crystallizes with a cubic unit cell of dimension and the space group Im3m. Refinement on F resulted in R=1.9%. The structure is comprised of a network of corners, edges and faces sharing the coordination polyhedra of neodymium. In between this skeleton the regular octahedra of oxygen-coordinated iron and trigonal prisms of lithium are located. The Mössbauer spectra revealed the presence of ▫$Fe^3+$▫, ▫$Fe^4+$▫ and ▫$Fe^5+$▫ ions distributed on two symmetry-independent lattice positions.
Keywords: crystal structure, ternary compounds, single-crystal X-ray diffraction, Mössbauer spectroscopy, iron oxidation state, kristalna struktura, ternarne spojine, rentgenska difrakcija, Mössbauerjeva spektroskopija, rentgenska strukturna analiza
Published: 01.06.2012; Views: 1658; Downloads: 38
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Subsolidus phase equilibria and the Li[sub]5Nd[sub]4FeO[sub]10 phase in the Li[sub]2O-Nd[sub]2O[sub]3-Fe[sub]2O[sub]3 system
Irena Ban, Mihael Drofenik, Danilo Suvorov, Darko Makovec, 2005, original scientific article

Abstract: A survey of the subsolidus phase equilibria in the system Li2O-Nd2O3-Fe2O3 wasmade at subsolidus temperatures in the range 1000-1050 °C. A ternary phase was identified. The phase is centered on Li5Nd4FeO10, with a cubic lattice a =11.9494 A. The compound melts incongruently at 1105 °C. The magnetic susceptibility was measured in the temperature range 4-300 K. The compound is paramagnetic in the temperature range 150-300 K and follows the Curie-Weiss law. At about TN = 10 K, a long-range magnetic ordering is observed.
Keywords: lithium ferrites, differential scanning calorimetry, thermogravimetric analysis, X-ray diffraction, magnetic properties, phase equilibrium
Published: 01.06.2012; Views: 1633; Downloads: 24
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Preparation of enantiomers using high pressure technologies
Paul Thorey, 2010, dissertation

Abstract: The study of two different methods of obtaining chiral alcohols is proposed herein. The requirement of the relatively new paradigm of green chemistry associated with clean technologies such as biocatalysis or non-conventional solvents, dense gases, was focused at. Indeed, the two methods of production of chiral alcohols were: - the conversion of acetophenone into (R)-1-phenylethanol in dense gases catalysed by Lactobacillus brevis alcohol dehydrogenase and its coenzyme, NADP/H; - the resolution of (±)-trans-1,2-cyclohexanediol by cocrystal formation with tartaric acid followed by supercritical extraction. In both cases high enantiopurities were achieved (ee>99%).
Keywords: High-pressure technologies, enantiomers, green chemistry, R-1-phenylethanol, Lactobacillus brevis, alcohol dehydrogenase, NADP, liquid propane, enzyme deactivation, resolution, trans-1, 2-cyclohexanediol, tartaric acid, cocrystal, supercritical carbon dioxide, extraction, X-ray diffraction, differential scanning calorimetry
Published: 02.02.2011; Views: 2391; Downloads: 88
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