scholarly journals Comparative Compressibility of Smectite Group under Anhydrous and Hydrous Environments

Materials ◽  
2020 ◽  
Vol 13 (17) ◽  
pp. 3784
Author(s):  
Yongmoon Lee ◽  
Pyosang Kim ◽  
Hyeonsu Kim ◽  
Donghoon Seoung
Keyword(s):  
High Pressure ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Environmental Changes ◽  
Silicone Oil ◽  
Distilled Water ◽  
X Ray ◽  
Water Conditions ◽  
Before And After ◽  
Cell Volumes

High-pressure synchrotron X-ray powder diffraction studies of smectite group minerals (beidellite, montmorillonite, and nontronite) reveal comparative volumetric changes in the presence of different fluids, as pressure transmitting media (PTM) of silicone oil and distilled water for anhydrous and hydrous environments at room temperature. Using silicone oil PTM, all minerals show gradual contraction of unit-cell volumes and atomistic interplane distances. They, however, show abrupt collapse near 1.0 GPa under distilled water conditions due to hydrostatic to quasi-hydrostatic environmental changes of water PTM around samples concomitant with the transition from liquid to ICE-VI and ICE-VII. The degrees of volume contractions of beidellite, montmorillonite, and nontronite up to ca. 3 GPa are ca. 6.6%, 8.9%, and 7.5% with bulk moduli of ca. 38(1) GPa, 31(2) GPa, and 26(1) GPa under silicone oil pressure, whereas 13(1) GPa, 13(2) GPa, and 17(2) GPa, and 17(1) GPa, 20(1) GPa, and 21(1) GPa under hydrostatic and quasi-hydrostatic environments before and after 1.50 GPa, respectively.

Synthesis of Superconducting Ceramics Hg0.82Re0.18Ba2Ca2Cu3O8+δ with Different Values of δ

2008 ◽  
Vol 591-593 ◽  
pp. 392-396 ◽  
Author(s):  
Luís Gallego Martinez ◽  
J.L. Rossi ◽  
M.T.D. Orlando ◽  
C.A.C. Passos ◽  
Francisco Cristóvão Lourenço de Melo ◽  
...  
Keyword(s):  
High Pressure ◽  
Diffraction Analysis ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Molar Ratio ◽  
High Tc ◽  
X Ray ◽  
Partial Pressures ◽  
Precursor Material ◽  
Superconducting Ceramics

Samples of the superconducting ceramics Hg0.82Re0.18Ba2Ca2Cu3O8+ were prepared by solid-vapor reaction technique. The preparation of the ceramic precursor started with a mixture of Ba2Ca2Cu3Ox and ReO2 powders with molar ratio 1:0.18. The precursor material was submitted to annealing under three different partial pressures of oxygen using a mixture of oxygen/argon at ratios: 5/95 (sample A), 10/90 (sample B) and 15/85 (sample C). X-ray powder diffraction analysis of the precursors identified the phases BaCuO2+x, Ba2Cu3O5+x, Ba4CaCu3O8+x, Ca2CuO3 and Ca5Re2O12 at different ratios in the samples, indicating an increment in the oxygen content from sample A to sample C. Finally, the precursors with different oxygen contents were blended with HgO at molar ratio 1:0.82 and treated in a sealed high pressure furnace to produce the high Tc superconducting ceramics. Rietveld refinement of XRD data showed differences in the crystal structures of the samples. The measurement of thermopower at room temperature resulted in distinct values, confirming the different oxygen sample doping.

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

Crystal structure of the anticancer drug carmustine determined by X-ray powder diffraction

2021 ◽  
pp. 1-3
Author(s):  
Carina Schlesinger ◽  
Edith Alig ◽  
Martin U. Schmidt
Keyword(s):  
Crystal Structure ◽  
Anticancer Drug ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Powder Diffraction Data ◽  
Orthorhombic Space Group ◽  
Commercial Sample ◽  
One Dimensional ◽  
X Ray ◽  
Hydrogen Bond Pattern

The structure of the anticancer drug carmustine (1,3-bis(2-chloroethyl)-1-nitrosourea, C5H9Cl2N3O2) was successfully determined from laboratory X-ray powder diffraction data recorded at 278 K and at 153 K. Carmustine crystallizes in the orthorhombic space group P212121 with Z = 4. The lattice parameters are a = 19.6935(2) Å, b = 9.8338(14) Å, c = 4.63542(6) Å, V = 897.71(2) ų at 153 K, and a = 19.8522(2) Å, b = 9.8843(15) Å, c = 4.69793(6) Å, V = 921.85(2) ų at 278 K. The Rietveld fits are very good, with low R-values and smooth difference curves of calculated and experimental powder data. The molecules form a one-dimensional hydrogen bond pattern. At room temperature, the investigated commercial sample of carmustine was amorphous.

Distorted chiolite crystal structures of α-Na5M3F14 (M=Cr,Fe,Ga) studied by X-ray powder diffraction

2003 ◽  
Vol 18 (2) ◽  
pp. 128-134 ◽  
Author(s):  
A. Le Bail ◽  
A.-M. Mercier
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Rietveld Refinements ◽  
Space Group ◽  
X Ray ◽  
Precise Characterization

The crystal structures of the chiolite-related room temperature phases α-Na5M3F14 (MIII=Cr,Fe,Ga) are determined. For all of them, the space group is P21/n, Z=2; a=10.5096(3) Å, b=7.2253(2) Å, c=7.2713(2) Å, β=90.6753(7)° (M=Cr); a=10.4342(7) Å, b=7.3418(6) Å, c=7.4023(6) Å, β=90.799(5)° (M=Fe), and a=10.4052(1) Å, b=7.2251(1) Å, c=7.2689(1), β=90.6640(4)° (M=Ga). Rietveld refinements produce final RF factors 0.036, 0.033, and 0.035, and RWP factors, 0.125, 0.116, and 0.096, for MIII=Cr, Fe, and Ga, respectively. The MF6 polyhedra in the defective isolated perovskite-like layers deviate very few from perfect octahedra. Subtle octahedra tiltings lead to the symmetry decrease from the P4/mnc space group adopted by the Na5Al3F14 chiolite aristotype to the P21/n space group adopted by the title series. Facile twinning precluded till now the precise characterization of these compounds.

Structural characterization of two K2SnX(PO4)3 (X=Fe,Yb) with langbeinite structure

2006 ◽  
Vol 21 (3) ◽  
pp. 214-219 ◽  
Author(s):  
Abderrahim Aatiq ◽  
Btissame Haggouch ◽  
Rachid Bakri ◽  
Youssef Lakhdar ◽  
Ismael Saadoune
Keyword(s):  
Solid State ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Cell Parameter ◽  
Rietveld Analysis ◽  
Conventional Solid State Reaction ◽  
X Ray ◽  
Octahedral Sites ◽  
Parameter Values

Structures of two K2SnX(PO4)3(X=Fe,Yb) phosphates, obtained by conventional solid state reaction techniques at 950 °C, were determined at room temperature by X-ray powder diffraction using Rietveld analysis. The two materials exhibit the langbeinite-type structure (P213 space group, Z=4). Cubic unit cell parameter values are: a=9.9217(4) Å and a=10.1583(4) Å for K2SnFe(PO4)3 and K2SnYb(PO4)3, respectively. Structural refinements show that the two crystallographically independent octahedral sites (of symmetry 3) have a mixed Sn∕X (X=Fe,Yb) population although ordering is stronger in the Yb phase than in the Fe phase.

Spektralreines Bis(phthalocyaninato)protactinium(IV) / Spectroscopically Pure Bis(phthalocyaninato)protactinium(IV)

1980 ◽  
Vol 35 (5) ◽  
pp. 564-567 ◽  
Author(s):  
Franz Lux ◽  
Oskar F. Beck ◽  
Heinz Krauß ◽  
David Brown ◽  
Tze C. Tso
Keyword(s):  
Solid State ◽  
Temperature Profile ◽  
Powder Diffraction ◽  
Phthalic Acid ◽  
Room Temperature ◽  
X Ray ◽  
Derivative Spectroscopy ◽  
Solid State Spectrum

Abstract Spectroscopically pure PaPc2 has been prepared by reaction between PaI4 · 4 CH3CN and o-phthalic acid dinitrile in 1-chloronaphthalene followed by sublimation at 5 · 10-3 Pa in a temperature profile with three clearly defined zones (520 °C/350 °C/room temperature). This procedure gives a product almost completely free of H2Pc impurity which is known to have been present in previously reported complexes of the type AnPc2. Thus, the trace of H2Pc in the substance could only be detected by derivative spectroscopy. X-ray powder diffraction shows the compound to be isostructural with ThPc2 and UPc2. The ligand spectrum is typical of AnPc2 complexes, f-f Bands observed in a solid state spectrum provide additional proof that the compound is PaIV Pc2.

Structure determination of the 1/1 α/β mixed lactose by X-ray powder diffraction

2005 ◽  
Vol 61 (4) ◽  
pp. 455-463 ◽  
Author(s):  
Jacques Lefebvre ◽  
Jean-François Willart ◽  
Vincent Caron ◽  
Ronan Lefort ◽  
Frédéric Affouard ◽  
...  
Keyword(s):  
Powder Diffraction ◽  
Size Effects ◽  
Room Temperature ◽  
Real Space ◽  
Hydroxyl Groups ◽  
Soft Constraints ◽  
Rietveld Refinements ◽  
X Ray ◽  
Mixed Compound

The mixed form of α/β lactose was obtained by heating amorphous α-lactose at 443 K. NMR spectroscopy determined the stoichiometry of this mixed compound to be 1/1. The X-ray powder diffraction pattern was recorded at room temperature with a sensitive curved detector (CPS 120). The structure was solved by real-space methods (simulated annealing) followed by Rietveld refinements with soft constraints on bond lengths and bond angles. The H atoms of the hydroxyl groups were localized by minimization of the crystalline energy. The cell of 1/1 α/β lactose is triclinic with the space group P1 and contains two molecules (one molecule of each anomer). The crystalline cohesion is achieved by networks of O—H...O hydrogen bonds. The width of the Bragg peaks is interpreted through a microstructural approach in terms of isotropic strain effects and anisotropic size effects.

The crystal structures of solvent-free alkali-metal squarates from powder diffraction data

2005 ◽  
Vol 220 (11) ◽  
Author(s):  
Robert E. Dinnebier ◽  
Hanne Nuss ◽  
Martin Jansen
Keyword(s):  
High Resolution ◽  
Alkali Metal ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Room Temperature ◽  
Solvent Free ◽  
Crystallographic Data ◽  
Powder Diffraction Data ◽  
X Ray

AbstractThe crystal structures of solvent-free lithium, sodium, rubidium, and cesium squarates have been determined from high resolution synchrotron and X-ray laboratory powder patterns. Crystallographic data at room temperature of Li

Preparation and Properties of Nano-Crystalline Cellulose Electro-Rheological Fluid

2015 ◽  
Vol 815 ◽  
pp. 217-221
Author(s):  
Ling Li Xu ◽  
Xing Ling Shi ◽  
Qing Liang Wang
Keyword(s):  
Room Temperature ◽  
Silicone Oil ◽  
Strong Acid ◽  
Crystalline Cellulose ◽  
Methyl Silicone ◽  
Shearing Stress ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nano Crystalline ◽  
Transmission Electron

nanocrystalline cellulose (NCC) was prepared from micro-crystalline cellulose (MCC) by strong acid hydrolysis. The characteristics of such particle were studied by transmission electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopy. Electro-rheological fluids (ERF) were prepared by dispersing NCC and MCC in methyl-silicone oil, and their ER effects were measured. Experimental results indicated that NCC ERF exhibited a remarkable ER effect. The highest static shearing stress of NCC ERF (3.5 g/ml) was 5.1 kPa at the room temperature under a 4 .2 kV/mm electric field, increased about 5.5 times compared to MCC ERF, and sedimentation of NCC ERF was not observed even after 60 days.

Structure determination of the stable anhydrous phase of α-lactose from X-ray powder diffraction

2005 ◽  
Vol 61 (2) ◽  
pp. 185-191 ◽  
Author(s):  
Cyril Platteau ◽  
Jacques Lefebvre ◽  
Frederic Affouard ◽  
Jean-François Willart ◽  
Patrick Derollez ◽  
...  
Keyword(s):  
Powder Diffraction ◽  
Room Temperature ◽  
Structural Model ◽  
Hydroxyl Groups ◽  
Rietveld Refinements ◽  
X Ray ◽  
Hydrogen Bond Networks ◽  
Monte Carlo Simulated Annealing ◽  
Annealing Method

The stable anhydrous form of α-lactose has been obtained by the dehydration of α-lactose monohydrate in methanol. An X-ray powder diffraction pattern was recorded at room temperature with a laboratory diffractometer equipped with an INEL curved sensitive detector CPS120. The starting structural model of this form was found by a Monte-Carlo simulated annealing method. The structure was obtained through Rietveld refinements and the minimization of crystalline energy for the localization of the H atoms of the hydroxyl groups. Soft restraints were applied to bond lengths and angles. Networks of O—H...O hydrogen bonds account for the crystalline cohesion. A comparison is made between the hydrogen-bond networks of this form and those of the monohydrate and hygroscopic anhydrous forms of α-lactose.

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