Search results for "Powder diffraction"
showing 10 items of 243 documents
Melting behaviour of d-sucrose, d-glucose and d-fructose
2004
The melting behaviour of d-sucrose, d-glucose and d-fructose was studied. The melting peaks were determined with DSC and the start of decomposition was studied with TG at different rates of heating. In addition, melting points were determined with a melting point apparatus. The samples were identified as d-sucrose, alpha-d-glucopyranose and beta-d-fructopyranose by powder diffraction measurements. There were differences in melting between the different samples of the same sugar and the rate of heating had a remarkable effect on the melting behaviour. For example, T(o), DeltaH(f) and T(i) (initial temperature of decomposition) at a 1 degrees Cmin(-1) rate of heating were 184.5 degrees C, 126…
The effect of Fe doping on superconductivity in ZrRuP
2011
Abstract This work reports the structure and superconducting properties of the superconductor ZrRuP doped with Fe; the ZrRu 1− x Fe x P solid solution was investigated by means of X-ray powder diffraction, SQUID magnetometry and Mosbauer spectroscopy. It is shown that the modification of the superconducting properties by doping with Fe is similar to the effect of chemical pressure and that the Fe doped compounds do not show any magnetic ordering.
Electron Crystallography in Mineralogy and Materials Science
2006
The mineral aerinite is investigated by electron crystallography (NED and HREM). TEM results of aerinite are compared with X-ray and synchrotron powder diffraction data. Six selected area electron diffraction (SAED) patterns and two HREM images from Pb5MoO8 single crystals are used to solve their structure. The unit cell parameters of these crystals confirm the known powder diffraction data.
Thermal and X-ray powder diffraction studies of aliphatic polyester dendrimers
2004
The syntheses and thermal and X-ray powder diffraction analyses of three sets of aliphatic polyester dendrimers based on 2,2-bis(hydroxymethyl)propionic acid as a repeating unit and 2,2-dimethyl-1,3-propanediol, 1,5-pentanediol, and 1,1,1-tris(hydroxymethyl)ethane as core molecules are reported. These dendritic polyesters were prepared in high yields with the divergent method. The thermal properties of these biodendrimers were evaluated with thermogravimetric analysis and differential scanning calorimetry. The thermal decomposition of the compounds occurred around 250 °C for the hydroxyl-ended dendrimers and around 150 °C for the acetonide-protected dendrimers. In addition, the crystallinit…
Elucidating Gating Effects for Hydrogen Sorption in MFU-4-Type Triazolate-Based Metal-Organic Frameworks Featuring Different Pore Sizes
2011
A highly porous member of isoreticular MFU-4-type frameworks, [Zn(5)Cl(4)(BTDD)(3)] (MFU-4l(arge)) (H(2)-BTDD=bis(1H-1,2,3-triazolo[4,5-b],[4',5'-i])dibenzo[1,4]dioxin), has been synthesized using ZnCl(2) and H(2)-BTDD in N,N-dimethylformamide as a solvent. MFU-4l represents the first example of MFU-4-type frameworks featuring large pore apertures of 9.1 Å. Here, MFU-4l serves as a reference compound to evaluate the origin of unique and specific gas-sorption properties of MFU-4, reported previously. The latter framework features narrow-sized pores of 2.5 Å that allow passage of sufficiently small molecules only (such as hydrogen or water), whereas molecules with larger kinetic diameters (e.…
Estimation of hydrogen transfer mechanisms in composite materials
2008
Abstract Spill-over effect as a hydrogen transfer mechanism is proposed to explain an increased capacity of hydrogen absorption and improvement of hydrogen activation kinetics in composite material based on the AB5 type metal hydride and powdered glass. A raw lanthanum nickel alloy AB5 with small amount of additives was used as catalyst and bulk material for hydrogen storage, and a borosilicate glass powder with developed surface was applied as a support material. Thermogravimetric technique to determine an absorbed amount of the hydrogen in materials and X-ray powder diffraction analysis for structural investigations was used.
A new approach to the synthesis of intermetallic compounds: mild synthesis of submicrometric CoxMy (M = Mo, W; x∶y = 3∶1 and 7∶6) particles by direct…
2002
A simple processing route to cobalt–molybdenum and cobalt–tungsten intermetallics (CoxMy, where M = Mo and W, and x∶y = 3∶1 and 7∶6) has been developed, on the basis of the use of precursors resulting from freeze-drying of aqueous solutions of the appropriate common metal salts. The influence of the preparative variables on the outcomes of this procedure is examined. These compounds are prepared as single phases by thermal reduction of amorphous freeze-dried powders under a hydrogen–argon atmosphere (8% H2), followed by slow cooling of the samples. The materials have been characterised by X-ray powder diffraction, metal analysis, scanning electron microscopy and thermogravimetry under an ox…
Synthesis of new vanadium–chromium and chromium–molybdenum oxynitrides by direct ammonolysis of freeze-dried precursors
2000
Interstitial vanadium–chromium and chromium–molybdenum oxynitrides in the solid solution series V1 − zCrz(OxNy) and Cr1 − zMoz(OxNy) (z = 0.0, 0.2, 0.4, 0.5, 0.6, 0.8, 1.0) have been obtained by direct ammonolysis of precursors resulting from the freeze-drying of aqueous solutions of the appropriate metal salts. A study of the influence of the preparative variables on the outcomes of this procedure is presented. Compounds in the V1 − zCrz(OxNy) series are prepared as single phases by nitridation at 1073 K, followed by fast cooling of the samples. Compounds in the Cr1 − zMoz(OxNy) series are prepared as nearly single phases by nitridation at different temperatures, optimized for each composi…
Time-Gated Raman Spectroscopy for Quantitative Determination of Solid-State Forms of Fluorescent Pharmaceuticals
2018
Raman spectroscopy is widely used for quantitative pharmaceutical analysis, but a common obstacle to its use is sample fluorescence masking the Raman signal. Time-gating provides an instrument-based method for rejecting fluorescence through temporal resolution of the spectral signal and allows Raman spectra of fluorescent materials to be obtained. An additional practical advantage is that analysis is possible in ambient lighting. This study assesses the efficacy of time-gated Raman spectroscopy for the quantitative measurement of fluorescent pharmaceuticals. Time-gated Raman spectroscopy with a 128 X (2) X 4 CMOS SPAD detector was applied for quantitative analysis of ternary mixtures of sol…
Compressibility and phase stability of iron-rich ankerite
2021
ABSTRACT: The structure of the naturally occurring, iron-rich mineral Ca₁․₀₈(₆)Mg₀.₂₄(₂)Fe₀.₆₄(₄)Mn₀.₆₄(₄)(CO₃)₂ ankerite was studied in a joint experimental and computational study. Synchrotron X-ray powder diffraction measurements up to 20 GPa were complemented by density functional theory calculations. The rhombohedral ankerite structure is stable under compression up to 12 GPa. A third-order Birch-Murnaghan equation of state yields V₀ = 328.2(3) ų, bulk modulus B₀ = 89(4) GPa, and its first-pressure derivative B'₀ = 5.3(8)-values which are in good agreement with those obtained in our calculations for an ideal CaFe(CO₃)₂ ankerite composition. At 12 GPa, the iron-rich ankerite structure …