Local environmental structures of Mo in the superionic conducting glass (AgI)(0.6)(Ag2MoO4)(0.4) by anomalous X-ray scattering

The anomalous X-ray scattering (AXS) method using Mo K absorption edges has been employed for obtaining the local structural information of superionic conducting glass having the composition (AgI)(0.6)(Ag2MoO4)(0.4). The possible atomic arrangements in the near-neighbor region of this glass were estimated by coupling the results with the least-squares variational analysis so as to reproduce the differential intensity profile for Mo as well as the ordinary scattering profile. The coordination number of oxygen around Mo is found to be about 4 at the distance of 0.180 mn. This implies that the most probable structural entity in the glass is the MoO4 tetrahedral unit which has been proposed based on infrared spectroscopy. The value of the coordination number of I- around Ag+ is estimated as 4.4 at 0.287 nm, suggesting an arrangement similar to that of crystalline or molten AgI.

Magneto-structural correlation in (mu-alkoxo/hydroxo)(mu-carboxylato)dicopper(II) systems: Synthesis, X-ray structure and magnetic properties of aquo(mu-hydroxo) (mu-arylcarboxylato)bis(N,N,N ',N '-tetramethylethane-1,2-diamine)dicopper(II) diperchlorate

Asymmetrically dibridged dicopper(II) complexes, [Cu-2(OH)(O2CC6H4-p-Me)(tmen)(2)(H2O)](ClO4)(2) (1) and [Cu-2(OH)(O2CC6H4-p-OMe)(tmen)(2)(H2O)](ClO4)(2) (2) (tmen = N,N,N',N'-tetramethylethane-1,2-diamine), were prepared and structurally characterized. Complex 1 crystallizes in the monoclinic space group P2(1)/a with a = 17.718(2), b = 9.869(1), c = 19.677(2) Angstrom, beta = 115.16(1)degrees, V = 3114.3(6) Angstrom(3) and Z = 4. The structure was refined to R(wR(2)) = 0.067(0.178). Complex 2 crystallizes in the monoclinic space group P2(1)/a with a = 17.695(3), b = 9.574(4), c = 20.104(2) Angstrom, beta = 114.18(1)degrees, V = 3107(1) Angstrom(3) and Z = 4. The final residuals are R(wR(2)) = 0.067(0.182). The complexes have a [Cu-2(mu-OH)(mu-OH)(mu-O2CAr)](2+) core with tmen Ligands occupying the terminal sites of the core. In addition, one copper is axially bound to a water molecule. The Cu ... Cu distances and the Cu-OH Cu angles in the core are 3.394(1) Angstrom, 124.4(2)degrees for 1 and 3.374(1) Angstrom, 123.3(3)degrees for 2. The complexes show axial X-band EPR spectral features in methanol glass at 77 K giving g(perpendicular to) = 2.02, g(parallel to) = 2.3 (A(parallel to) = 165 x 10(-4) cm(-1)) and a visible band near similar to 630 nm in methanol. The complexes are weakly antiferromagnetic. A theoretical fit of the magnetic susceptibility data in the temperature range 40-295 K gives -J = 10 cm(-1), g = 2.05 for 1 and -J = 10 cm(-1), g = 2.0 for 2. Plots of -2J versus the Cu-OH-Cu angle (phi) in this class of asymmetrically dibridged dicopper(II) complexes having d(x2-y2)-d(x2-y2) magnetic orbitals show a linear magneto-structural correlation: -2J(cm(-1)) = 11.48 phi(deg) - 1373.

Measurement of axial dispersion coefficient in a packed bed using X-ray

Dispersion of the liquid in a porous media is of great importance in many areas of engineering and has been studied by several researchers so far. A new experimental method has been developed to measure the dispersion coefficient. X-ray absorption technique provides a better understanding of dispersion that characterizes the mixing phenomenon in the packed beds. This is because the method is non-invasive and also it gives tracer concentration data at every point within the bed. The axial dispersion in a cylindrical bed of non-porous and non-wetting spherical particles has been measured for the flow of water. Aqueous barium chloride solution has been used a as tracer. X-ray images, recorded on a videocassette, have been analyzed using an image processing software to extract the local interstitial velocity and concentration data in the bed. Local dispersion coefficient has been determined with the help of aforementioned data. By using these data, the overall dispersion coefficient in a packed bed can also be estimated.

Crystallization of SrCO3 on a self-assembled monolayer substrate: an in-situ synchrotron X-ray study

Self-assembled monolayers (SAMs) of alkanethiols on gold surfaces show great promise in controlling the nucleation and growth of inorganic minerals from solution. In doing so, they mimic the role of some biogenic macromolecules in natural biomineralisation processes. Crystallization on SAM surfaces is usually monitored ex-situ; by allowing the process to commence and to evolve for some time, removing the substrate from the mother solution, and then examining it using microscopy, diffraction etc. We present here for the first time, the use of high energy monochromatic synchrotron X-radiation in conjunction with a two dimensional detector to monitor in situ, in a time resolved fashion, the growth of SrCO3 (strontianite) crystals on a SAM substrate.

A kinetic study of the phase transformations in Al2O3 and Na2O · 6Al2O3 by a combined use of 27Al MAS NMR spectroscopy and x-ray diffraction: Importance of nucleation

Phase transformations of Al2O3 and Na2O · 6Al2O3 prepared by the gel route have been investigated for the first time by 27Al MAS NMR spectroscopy in combination with x-ray diffraction. Of particular interest in the study is the kinetics of the γ → α and γ → β transformations, respectively, in these two systems. Analysis of the kinetic data shows the important role of nucleation in both these transformations.

Cloning, expression, purification and preliminary X-ray diffraction studies of a putative Mycobacterium smegmatis thiolase

Thiolases are important in fatty-acid degradation and biosynthetic pathways. Analysis of the genomic sequence of Mycobacterium smegmatis suggests the presence of several putative thiolase genes. One of these genes appears to code for an SCP-x protein. Human SCP-x consists of an N-terminal domain (referred to as SCP2 thiolase) and a C-terminal domain (referred as sterol carrier protein 2). Here, the cloning, expression, purification and crystallization of this putative SCP-x protein from M. smegmatis are reported. The crystals diffracted X-rays to 2.5 angstrom resolution and belonged to the triclinic space group P1. Calculation of rotation functions using X-ray diffraction data suggests that the protein is likely to possess a hexameric oligomerization with 32 symmetry which has not been observed in the other six known classes of this enzyme.

Novel double insertion of carbon disulfide into two Ru-H bonds of [(dppm)(2)Ru(H)(2)] (dppm = Ph2PCH2PPh2): Synthesis and crystal structure of a methanedithiolate complex

Addition of excess carbon disulfide to cis/trans-[(dPPM)(2)Ru(H)(2)] results in the methanedithiolate complex [(dppm)(2)Ru(eta(2)-S2CH2)] 4 via the intermediacy of cis-[(dppm)(2)Ru(H)(SC(S)H)] 2. The X-ray crystal structure of this species has been determined.

Structural changes in single-walled carbon nanotubes under non-hydrostatic pressures: x-ray and Raman studies

Using in situ x-ray diffraction and Raman scattering techniques, we have investigated the behaviour of single-walled carbon nanotubes bundles under non-hydrostatic pressures. It is seen that the diffraction line corresponding to the two-dimensional triangular lattice in the bundles is not reversible for pressures beyond 5 GPa, in sharp contrast to earlier results under hydrostatic pressure conditions. Most interestingly, radial breathing and tangential Raman modes of the pressure-cycled samples from 21 and 30 GPa match very well with those of the starting sample. Raman and x-ray results put together clearly suggest that the ordering of tubes in the bundles is only marginally regained with a very short coherence length on decompression.

Studies of the wetting characteristics of liquid iron on dense alumina by the X-ray sessile drop technique

In the present work, the reaction between a molten iron drop and dense alumina was studied using the X-ray sessile-drop method under different oxygen partial pressures in the gas atmosphere. The changes in contact angles between the iron drop and the alumina substrate were followed as functions of temperature and varying partial pressures of oxygen in the temperature range 1823 to 1873 K both in static and dynamic modes. The results of the contact angle measurements with pure iron in contact with dense alumina in extremely well-purified argon as well as under different oxygen partial pressures in the gas atmosphere showed good agreement with earlier measurements reported in the literature. In the dynamic mode, when argon was replaced by a CO-CO2-Ar mixture with a well-defined PO, in the gas, the contact angle showed an initial decrease followed by a period of nearly constant contact angle. At the end of this period, the length of which was a function of the P-O2 imposed, a further steep decrease in the contact angle was noticed. An intermediate layer of FeAl2O4 was detected in the scanning electron microscope (SEM) analysis of the reacted substrates. An interesting observation in the present experiments is that the iron drop moved away from the site of the reaction once the product layer covered the interface. The results are analyzed on the basis of the various forces acting on the drop.

The nature of the prompt X-ray and radio emission from SN 2002ap

We report on the combined X-ray and radio observations of the type Ic SN 2002ap, using XMM-Newton TOO observation of M 74 and the Giant Metrewave Radio Telescope ( GMRT). We account for the presence of a nearby source in the pre-supernova Chandra field of view in our measurements of the X-ray flux (0.3-10 KeV) 5.2 days after the explosion. The X-ray spectrum is well fitted by a power law spectrum with photon index alpha = 2.6. Our results suggest that the prompt X-ray emission originates from inverse Compton scattering of photospheric thermal emission by energetic electrons. Radio observations with the GMRT at 610 MHz (8 days after the explosion) and 1420 MHz (70 days after the explosion) are combined with the high frequency VLA observations of SN 2002ap reported by Berger et al. ( 2002), and the early radiospheric properties of SN 2002ap are compared with similar data from two other supernovae. Finally, the GMRT radio map reveals four other X-ray sources in the field of view of M 74 with radio counterparts.

Cold model study of local liquid holdup in the dropping zone using x-ray

It is important to know and to quantify the liquid holdups both dynamic and static at local levels as it will lead to understand various blast furnace phenomena properly such as slag/metal.gas.solid reactions, gas flow behaviour and interfacial area between the gas/solid/liquid. In the present study, considering the importance of local liquid holdup and non-availability of holdup data in these systems, an attempt has been made to quantify the local holdups in the dropping and around raceway zones in a cold model study using a non-wetting packing for liquid. In order to quantify the liquid holdups at microscopic level, a previously developed technique, X-ray radiography, has been used. It is observed that the liquid flows in preferred paths or channels which carry droplets/rivulets. It has been found that local holdup in some regions of the packed bed is much higher than average at a particular flow rate and this can have important consequences for the correct modelling of such systems.

X-ray structure of a galactose-specific lectin from Spatholobous parviflorous

A galactose-specific seed lectin from Spatholobous parviflorus (SPL) has been purified, crystallized and its X-ray structure solved. It is the first lectin purified and crystallized from the genus Spatholobus (family: Fabaceae). The crystals belong to the space group P1, with a = 60.792 angstrom, b = 60.998 angstrom, c = 78.179 angstrom, alpha = 78.68 degrees, beta = 88.62 degrees, gamma = 104.32 degrees. The data were collected at 2.04 angstrom resolution under cryocondition, on a MAR image-plate detector system, mounted on a rotating anode X-ray generator. The coordinates of Dolichos biflorus lectin (1lu1) were successfully used for the structure solution by molecular replacement method. The primary structure of the SPL was not known earlier and it was unambiguously visible in the electron density. S. parviflorus lectin is a hetero-dimeric-tetramer with two alpha and two beta chains of 251 and 239 residues respectively. SPL has two metal ions, Ca(2+) and Mn(2+), bound to a loop region of each chain. The SPL monomers are in jelly roll form. (C) 2011 Elsevier B.V. All rights reserved.