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PubMed2005

Synthesis of single-crystal gold nanosheets of large size in ionic liquids.

Large-size single-crystal gold nanosheets have been successfully prepared by microwave heating of HAuCl(4) in ionic liquid, 1-butyl-3-methylimidazolium tetrafluoroborate, without any additional template agent. Transmission electron microscopy (TEM), electron diffraction (ED), scanning electron microscopy (SEM), and X-ray powder diffraction (XRD) were used to characterize the resultant gold nanosheets. It was demonstrated that the ionic liquid could act as template agent for the formation of gold nanosheets. The present synthesis route is very simple and fast. It can be expected that the method can be extended to the fabrication of other metal nanosheets in ionic liquids.

Journal Article↗
PubMed1988

The effect of hydroxyapatite crystallinity on hemolysis.

Crystalline hydroxyapatite is a component of bone, teeth, and numerous pathological calcifications. The apatite crystal structure can accommodate a wide variety of atomic substitutions which gives apatite crystals an unusually high degree of variability in biochemical and physical properties. Apatite crystallites interact with numerous cellular systems in vivo, and some of these interactions may lead to altered cellular function. One measure of crystal-membrane interactions is crystal-induced membranolysis of human red blood cells. Hemolytic potentials at constant crystal surface areas were measured at 1, 2, and 4 hours for 29 different preparations of apatite. Each apatite sample was characterized by its morphology, particle size, % CO3, zeta potential, and broadening of the (211), (112), (300), (202), and (002) diffraction maxima. Only the surface area/g and the X-ray powder diffraction line broadening showed a significant inverse correlation with hemolytic potential. These parameters were related to each other, and are indications of the degree of crystallinity.

Crystallization↗
PubMed2000

Anharmonicity of potentials of atoms in potassium hydrogensulfide (KDS) determined by neutron single-crystal diffraction

Potassium hydrogensulfide (KHS) is an ionic compound with an anionic molecular group HS(-). The fast reorientational disorder of the anions was determined for the ambient temperature modification [R3;m; Jeffrey (1974). Can. J. Phys. 52, 2370-2378]. Single crystals are available now as protonated or deuterated specimens. With neutron single-crystal diffraction at room temperature, a considerable anharmonicity of the atom potential of the H or D atoms was observed. Even the thermal motions of K and S atoms show small deviations from an isotropic probability density function, which can be modelled using anharmonic temperature factors. The temperature factors of the atoms were expanded into a Gram-Charlier series [Kuhs (1992). Acta Cryst. A48, 80-98] in order to evaluate the anharmonicity quantitatively. Parameters up to a fourth-order approximation are relevant for the D atoms. Results from neutron single-crystal diffraction are compared with split-atom models extracted from neutron powder diffraction patterns of fully deuterated samples.

Journal Article↗
PubMed2004

Electrochemical deposition of platinum nanoparticles on carbon: a study by standard and anomalous X-ray diffraction.

This paper is devoted to an alternative method to characterize platinum nanoparticles: X-ray powder diffraction with synchrotron radiation in classical and anomalous dispersion modes. We could straightforwardly determine the mean diameter and the surface concentration of carbon-supported platinum nanoparticles, even down to diameters of 2-3 nm and catalyst amounts of 0.03 mgcm(-2). We could study early stages of the formation of electrochemically prepared platinum nanoparticles from [PtCl4(2-) species preadsorbed on carbon inside a carbon-Nafion layer, to obtain a fuel-cell electrode. Our X-ray diffraction (XRD) results demonstrate that, provided the superficial concentration is not too high, new and smaller particles appear for each current pulse, since there is not any strong nucleation limitation for the high overvoltages obtained. Hydrogen evolution becomes the main electrochemical phenomenon on particles of sufficient size and it explains the noteworthy size limitation. Better yields of Pt metal are obtained for smaller current densities and longer times: the rate-determining step is then not electrochemical, but chemical or related to superficial diffusion.

Journal Article↗
PubMed2003

Neutron diffraction study of the size-induced tetragonal to monoclinic phase transition in zirconia nanocrystals.

Accurate neutron powder diffraction experiments at several temperatures allow one to monitor the reconstructive tetragonal to monoclinic phase transition as a function of the size of zirconia nanoparticles. The structure of the tetragonal phase observed in the nanocrystals is identical to that observed in micrometric zirconia above 1400 K. A uniaxial strain depending on grain size is observed. The phase transition occurs above a threshold crystal size. These results are analyzed within the Landau theory and can be understood as a mechanism of size-dependent phase transition where the primary order parameter is altered by the nanoparticle size.

Journal Article↗
PubMed2005

Photoluminescence properties and analysis of spectral structure of Eu3+-doped SrY2O4.

The aim of this work is to report on the luminescence properties of SrY2O4 activated by Eu3+ ion. Powder samples were prepared by solid-state reaction. X-ray diffraction powder data, photoluminescence, and high-resolution spectroscopy were carried out. Results revealed that the Eu3+ ions occupied three nonequivalent sites, with one at the Sr site, one at the Y(1) site, and another at the Y(2) site. Their spectra wavelengths for the 7F0-5D0 transition are located at 578.49, 581.86, and 580.63 nm, respectively. The corresponding charge-transfer transitions are located at 248, 257, and 270 nm, respectively, which are also confirmed by theoretical analysis.

Journal Article↗
PubMed2006

Low-temperature phases of rubidium silver iodide: crystal structures and dynamics of the mobile silver ions.

Recently, broad-band conductivity spectra have been taken in the low-temperature gamma-phase of the archetypal fast ion conductor RbAg4I5. Attempts to reproduce the experimental data in a simple model calculation have led to the conclusion that strictly localized displacive movements of interacting ionic charge carriers should play an important role in the low-temperature phase. However, with no detailed structural study of gamma-RbAg4I5 available, the relevant processes could not be identified within the crystal structure. This state of affairs has triggered the present investigation of the structures of all three phases of rubidium silver iodide. Powder diffraction data of RbAg4I5 have been collected at the high-resolution powder diffractometer at ID31 at the European Synchrotron Radiation Facility (ESRF). The structure of the gamma-phase has been solved by successive Rietveld refinements in combination with difference Fourier analyses. The same structural principle is found to prevail in all three phases, interconnected distorted RbI6 octahedra forming a three-dimensional framework, which undergoes only displacive structural changes during the alpha-beta and beta-gamma phase transitions. With decreasing temperature, the disorder in the silver sublattice is found to decrease, and a clustering of the disordered silver ions is found to develop. In the gamma-phase, "pockets" containing partially occupied silver sites have been identified, and it is suggested that the localized displacive motion detected by conductivity spectroscopy is performed by the silver ions located within these pockets.

Journal Article↗
PubMed2000

Dissolution properties of piroxicam powders and capsules as a function of particle size and the agglomeration of powders.

The poor dissolution characteristics of relatively insoluble drugs have long been a problem to the pharmaceutical industry. An example is piroxicam, a highly potent anti-inflammatory agent. In many countries, a large number of generic piroxicam products are available to the prescriber. The aim of this study was to investigate the cause of the dissolution problems experienced by manufacturers of generic piroxicam capsules. Two raw material batches and the dissolution properties of several piroxicam capsules were studied. Differential scanning calorimetry (DSC) and X-ray powder diffraction (XRPD) results showed that the two raw material samples were identical with respect to polymorphic modification. The particles of powder 1 were smaller than those of powder 2, but the dissolution of powder 1 was much slower than that of powder 2. The dissolution results for the capsules showed a marked difference among different brands, with capsule C not meeting the USP tolerance. Adding surfactant to the dissolution medium increased the dissolution of both powder 1 and capsule C. Failure of powder 1 or capsule C to meet USP dissolution criteria could result in differences in product efficacy, as well as in potential side effects. Such observations should be taken into account along with other relevant considerations when decisions regarding the generic substitution of oral piroxicam products are made.

Administration, Oral↗
PubMed1981

Analysis of renal calculi by X-ray diffraction and electron microprobe: a comparison of two methods.

We analyzed 48 renal calculi by X-ray powder diffraction and electron microprobe techniques. In 35 of these, the presence of a minor constituent, not detected by X-ray diffraction, was revealed--hydroxyapatite was found in 24 stones, struvite in 6, and calcium oxalate in 5. The results of this study, as well as others, show that incomplete assignment of the crystalline constituents of urinary calculi is an inherent risk of the X-ray method and that conclusions concerning total chemical composition should be based on X-ray diffraction analyses coupled with data obtained from other analytical procedures.

Calcium Oxalate↗
PubMed1999

Effect of powder grinding on hydroxyapatite formation in a polymeric calcium phosphate cement prepared from tetracalcium phosphate and poly(methyl vinyl ether-maleic acid).

The primary aim of this study was to determine if cements based on poly(methyl vinyl ether-maleic acid) (PMVE-Ma) and tetracalcium phosphate resulted in hydroxyapatite formation. In addition, the mechanical strength of this type of polymeric calcium phosphate cement was evaluated. Cements were prepared by mixing, in a powder/liquid mass ratio of 3.0, an aqueous solution of PMVE-Ma (mass fraction = 25%) and tetracalcium phosphate powders ground for various periods of time. The tetracalcium phosphate powders and set cements were characterized by means of X-ray powder diffraction and scanning electron microscopy. Mechanical strengths of the cements were tested 24 h after mixing. Prolonged grinding of tetracalcium phosphate powder decreased particle size and/or crystallite size and increased lattice distortion. This enhanced the reactivity of the tetracalcium phosphate powder and elevated the extent of crosslinking between PMVE-Ma molecules, resulting in improved mechanical strength. Hydroxyapatite formation was detected in the cement prepared with the most finely ground tetracalcium phosphate powder. The conversion of residual tetracalcium phosphate particles to more thermodynamically stable hydroxyapatite crystals will reduce the solubility of the polymeric cement and increase its biocompatibility.

Calcium Phosphates↗
PubMed1988

Crystallographic modelling.

The project on crystallographic modelling aims at extending the application of interactive graphics to inorganic structures. Starting from the available expertise in organic and protein modelling, the symmetry of the crystal structure is used not only to draw fixed models of many unit cells of the structure, which as an entity can be interactively manipulated, but also to change details of the structures interactively with retention of the original symmetry. Real-time shifts of atom positions are automatically applied to all symmetry-equivalent atoms given the symmetry constraints. This also applies to translations and rotations of groups of atoms. In order to get feedback about these structural changes one can simulate powder diffraction patterns in real-time mode and compare them with the experimental powder patterns. These features are crucial in truly crystallographic modelling, but have not been implemented before in other programs. The program can be used in combination with standard molecular modelling programs and is also interfaced to the Inorganic Crystal Structure Database. Before describing the realization of these features on state-of-the-art hardware, we will review the expertise in molecular modelling and discuss an MS-DOS program to study inorganic crystal structures.

Computer Graphics↗
PubMed2006

Controllable assembly of metal-directed coordination polymers under diverse conditions: a case study of the M(II)-H3tma/Bpt mixed-ligand system.

A series of new metal-organic polymeric complexes, [[Co(bpt)(Htma)(H2O)3].2.25H2O]n (1), [Co(bpt)(Htma)(H2O)]n (2), [Ni(bpt)(Htma)(H2O)]n (3), [Zn(bpt)2(H2tma)2].6H2O (4), [[Cd(bpt)(Htma)(H2O)].(C2H5OH)(H2O)1.5]n (5), and [[Cd(bpt)(Htma)(H2O)2].5.5H2O]n (6), was prepared from solution reactions of 4-amino-3,5-bis(4-pyridyl)-1,2,4-triazole (bpt) and trimesic acid (H3tma) with different metal salts under diverse conditions. All these compounds were structurally determined by X-ray single-crystal diffraction, and the bulk new materials were further identified by X-ray powder diffraction. Complexes 1 and 6 show 1-D zigzag or linear Htma-bridged polymeric chains, with the terminal bpt ligands as pendants, which are extended to 2-D hydrogen-bonded arrays with 4.8(2) or (6,3) network topology. Coordination polymers 2 and 3, in which the 2-D corrugated metal-organic frameworks make the interdigitated 3-D packing, are isostructural. Complex 4 has a mononuclear structure, and its subunits are hydrogen-bonded to each other to give a 2-D grid-like net. For complex 5, the Cd(II) centers are linked by bpt/Htma ligands to form a 2-D (4,4) coordination layer, and these layers are interdigitated in pairs. Notably, secondary noncovalent forces, such as hydrogen bonds, play an important role in extending and stabilizing these structural topologies. Interestingly, distinct products are obtained for Co(II) (1 and 2) and Cd(II) (5 and 6) under ambient or hydrothermal conditions; however, for Ni(II) and Zn(II), single products, 3 and 4, are generated. The thermal stabilities of 1-6 were studied by thermogravimetric analysis of mass loss. The desorption/adsorption properties of the porous material 5 are also discussed. Solid-state luminescent spectra of the Zn(II) and Cd(II) complexes, 4-6, indicate intense fluorescent emissions at ca. 380 nm.

Journal Article↗
PubMed2006

Controlled synthesis of Ag/TiO2 core-shell nanowires with smooth and bristled surfaces via a one-step solution route.

Ag/TiO2 core-shell nanowires were synthesized via a one-step solution method without using a template. Interestingly, the shell morphologies can be controlled to be smooth or bristled by altering the reaction temperature. Moreover, the TiO2 shell thickness and bristle length can be tuned by changing the AgNO3 concentration. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electron diffraction (SAED), energy-dispersive X-ray analysis (EDS), X-ray powder diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) were used to characterize the resultant Ag/TiO2 core-shell nanowires. Moreover, the absorption peaks of our samples are significantly red-shifted compared with those of the uncoated pure silver nanowires, indicating that interaction between the core and shell occurred. On the basis of the experimental results, we proposed a template-induced Oswald ripening mechanism to explain the formation of the Ag/TiO2 core-shell nanowires.

Journal Article↗
PubMed1999

The effect of formulation excipients on protein stability and aerosol performance of spray-dried powders of a recombinant humanized anti-IgE monoclonal antibody.

PURPOSE: To study the effect of trehalose, lactose, and mannitol on the biochemical stability and aerosol performance of spray-dried powders of an anti-IgE humanized monoclonal antibody. METHODS: Protein aggregation of spray-dried powders stored at various temperature and relative humidity conditions was assayed by size exclusion chromatography and sodium dodecyl sulfate polyacrylamide gel electrophoresis. Protein glycation was determined by isoelectric focusing and affinity chromatography. Crystallization was examined by X-ray powder diffraction. Aerosol performance was assessed as the fine particle fraction (FPF) of the powders blended with coarse carrier lactose, and was determined using a multiple stage liquid impinger. RESULTS: Soluble protein aggregation consisting of non-covalent and disulfide-linked covalent dimers and trimers occurred during storage. Aggregate was minimized by formulation with trehalose at or above a molar ratio in the range of 300: 1 to 500:1 (excipient:protein). However, the powders were excessively cohesive and unsuitable for aerosol administration. Lactose had a similar stabilizing effect, and the powders exhibited acceptable aerosol performance, but protein glycation was observed during storage. The addition of mannitol also reduced aggregation, while maintaining the FPF, but only up to a molar ratio of 200:1. Further increased mannitol resulted in crystallization, which had a detrimental effect on protein stability and aerosol performance. CONCLUSIONS: Protein stability was improved by formulation with carbohydrate. However, a balance must be achieved between the addition of enough stabilizer to improve protein biochemical stability without compromising blended powder aerosol performance.

Aerosols↗
PubMed2002

Terephthalate salts of dipositive cations.

The crystal structures of M(C(8)H(4)O(4))(H(2)O)(2), M = Mg, Mn, Fe and Co, have been determined by applying Monte Carlo simulated annealing techniques to synchrotron powder diffraction data and refined by the Rietveld method using both synchrotron and laboratory powder data. These isostructural compounds crystallize in the monoclinic space group C2/c, with 18.2734 (9) <or= a <or= 18.7213 (13), 6.5186 (13) <or= b <or= 6.5960 (4), 7.2968 <or= c <or= 7.4034 (6) A, 98.653 (2) <or= beta <or= 99.675 (1) degrees and Z = 4. The structure consists of alternating layers (perpendicular to a) of terephthalate anions and octahedrally coordinated metal cations. The octahedra are isolated; each carboxylate bridges two metal cations. The equatorial metal coordination consists of four terephthalate O atoms and there are two axial water molecules. Both water-molecule H atoms participate in normal-strength hydrogen bonds to carboxylate O atoms. Quantum chemical calculations (using CASTEP) were used to determine the H-atom positions and analyze the hydrogen bonding and the metal coordination. Both the atomic charges and the M-O bond-overlap populations indicate that, despite the fact that these compounds are isostructural, the metal-terephthalate bonding is different. The bonding in the Mg complex is essentially ionic, while the M-O bonds in the Mn, Fe and Co complexes have significant covalent character. Comparison of a new Rietveld refinement of the structure of copper(II) terephthalate trihydrate with the reported single-crystal structure provides an opportunity to assess the accuracy and precision that can be expected from structures of aromatic carboxylates determined using X-ray powder data. The average difference between the bond distances in the two structures is 0.03 A and the average difference in bond angles is only 1.1 degrees.

Journal Article↗
PubMed2003

X-ray and neutron diffraction studies on "Li4.4Sn".

A chemical analysis and detailed structural characterization, using X-ray single crystal and neutron powder diffraction, of the binary lithium-tin compound "Li(4.4)Sn" is presented. Phase analyses and subsequent structural refinements result in the reformulation of "Li(4.4)Sn" as Li(17)Sn(4). The lithium-rich binary phase crystallizes with a complex cubic structure in the space group Ffourmacr;3m, with a = 19.6907(11) A, Z = 20. The improved crystal structure determination indicates well-defined lithium atom positions, some of which differ from those previously reported. The nearly Zintl phase Li(17)Sn(4) exhibits poor metallic behavior similar to that of heavily doped semiconductors. Comparisons of the refined crystal structure with previously reported X-ray crystal structures associated with "Li(4.4)Sn" are discussed.

Journal Article↗
PubMed2006

In vitro biocompatibility of a novel Fe2O3 based glass ionomer cement.

INTRODUCTION: Since their invention in the late 1960s, glass ionomer cements (GICs) have been used extensively in dentistry but recently they have also been utilised in ear nose and throat (ENT) surgery. Unfortunately, Al3+, a component of conventional ionomer glasses, has been linked to poor bone mineralisation and neurotoxicity. OBJECTIVE: The aim of the research was to modify a commercial ionomer glass composition by substituting Al2O3 with Fe2O3. METHODS: Glasses with the following molar compositions were fabricated: 4.5SiO2*3M2O3*XP2O5*3CaO*2CaF2 (M = Al or Fe, X = 0-1.5). The glasses were characterised using X-ray fluorescence (XRF) and X-ray powder diffraction (XRD). Cements were prepared using a standard ratio of; 1 g of glass powder: 0.2 g of dried polyacrylic acid: 0.3 g of 10% tartaric acid solution. Cement formation was assessed using a Gilmore needle and in vitro biocompatibility was investigated for novel cement formulations. RESULTS: XRF revealed that the Fe2O3-based glasses had Al2O3 contamination from the crucibles and also had undergone substantial F- losses. XRD gave peaks that corresponded to magnetite Fe3O4 (JCPDS # 19-629) in all compositions. Apatite Ca5(PO4)3(OH,F) (JCPDS # 15-876) was identified in P2O5 containing glasses. It was possible to fabricate cements from all of the Fe2O3-based ionomer glasses. Good in vitro biocompatibility was observed for the Fe2O3-based cements. CONCLUSION: Ionomer glasses may be prepared by entirely replacing Al2O3 with Fe2O3. Cement setting times appeared to be related to P2O5 content. Fe2O3-based cements showed good in vitro biocompatibility.

Animals↗