Crystallization and preliminary X-ray diffraction analysis of a novel Arg49 phospholipase A(2) homologue from Zhaoermia mangshanensis venom

Zhaoermiatoxin, an Arg49 phospholipase A(2) homologue from Zhaoermia mangshanensis (formerly Trimeresurus mangshanensis, Ermia mangshanensis) venom is a novel member of the PLA(2)-homologue family that possesses an arginine residue at position 49, probably arising from a secondary Lys49 -> Arg substitution that does not alter the catalytic inactivity towards phospholipids. Like other Lys49 PLA(2) homologues, zhaoermiatoxin induces oedema and strong myonecrosis without detectable PLA(2) catalytic activity. A single crystal with maximum dimensions of 0.2 x 0.2 x 0.5 mm was used for X-ray diffraction data collection to a resolution of 2.05 angstrom using synchrotron radiation and the diffraction pattern was indexed in the hexagonal space group P6(4), with unit-cell parameters a = 72.9, b = 72.9, c = 93.9 angstrom.

An approach to three-dimensional structures of biomolecules by using single-molecule diffraction images

We describe an approach to the high-resolution three-dimensional structural determination of macromolecules that utilizes ultrashort, intense x-ray pulses to record diffraction data in combination with direct phase retrieval by the oversampling technique. It is shown that a simulated molecular diffraction pattern at 2.5-Å resolution accumulated from multiple copies of single rubisco biomolecules, each generated by a femtosecond-level x-ray free electron laser pulse, can be successfully phased and transformed into an accurate electron density map comparable to that obtained by more conventional methods. The phase problem is solved by using an iterative algorithm with a random phase set as an initial input. The convergence speed of the algorithm is reasonably fast, typically around a few hundred iterations. This approach and phasing method do not require any ab initio information about the molecule, do not require an extended ordered lattice array, and can tolerate high noise and some missing intensity data at the center of the diffraction pattern. With the prospects of the x-ray free electron lasers, this approach could provide a major new opportunity for the high-resolution three-dimensional structure determination of single biomolecules.

Experiments and analysis of combined diffraction and self diffraction effects in a nematic liquid crystal cell

The potential for nonlinear optical processes in nematic-liquid-crystal cells is great due to the large phase changes resulting from reorientation of the nematic-liquid-crystal director. Here the combination of diffraction and self-diffraction effects are studied simultaneously by the use of a pair of focused laser beams which are coincident on a homeotropically aligned liquid-crystal cell. The result is a complicated diffraction pattern in the far field. This is analyzed in terms of the continuum theory for liquid crystals, using a one-elastic-constant approximation to solve the reorientation profile. Very good comparison between theory and experiment is obtained. An interesting transient grating, existing due to the viscosity of the liquid-crystal material, is observed in theory and practice for large cell-tilt angles.

Observations of diffraction and self diffraction effects during two wave mixing in a nematic liquid crystal

We report observations of the diffraction pattern resulting when a nematic liquid crystal is illuminated with two equal power, high intensity beams of light from an Ar+ laser. The time evolution of the pattern is followed from the initial production of higher diffraction orders to a final striking display arising as a result of the self-diffraction of the two incident beams. The experimental results are described with good approximation by a model assuming a phase distribution at the output plane of the liquid crystal in the form of the sum of a gaussian and a sinusoid.

Observations of diffraction and self diffraction effects during two wave mixing in a nematic liquid crystal

We report observations of the diffraction pattern resulting when a nematic liquid crystal is illuminated with two equal power, high intensity beams of light from an Ar+ laser. The time evolution of the pattern is followed from the initial production of higher diffraction orders to a final striking display arising as a result of the self-diffraction of the two incident beams. The experimental results are described with good approximation by a model assuming a phase distribution at the output plane of the liquid crystal in the form of the sum of a gaussian and a sinusoid.

Experiments and analysis of combined diffraction and self diffraction effects in a nematic liquid crystal cell

The potential for nonlinear optical processes in nematic-liquid-crystal cells is great due to the large phase changes resulting from reorientation of the nematic-liquid-crystal director. Here the combination of diffraction and self-diffraction effects are studied simultaneously by the use of a pair of focused laser beams which are coincident on a homeotropically aligned liquid-crystal cell. The result is a complicated diffraction pattern in the far field. This is analyzed in terms of the continuum theory for liquid crystals, using a one-elastic-constant approximation to solve the reorientation profile. Very good comparison between theory and experiment is obtained. An interesting transient grating, existing due to the viscosity of the liquid-crystal material, is observed in theory and practice for large cell-tilt angles.

Near-field diffraction of chirped gratings

In this Letter, we analyze the near-field diffraction pattern produced by chirped gratings. An intuitive analytical interpretation of the generated diffraction orders is proposed. Several interesting properties of the near-field diffraction pattern can be determined, such as the period of the fringes and its visibility. Diffraction orders present different widths and also, some of them present focusing properties. The width, location, and depth of focus of the converging diffraction orders are also determined. The analytical expressions are compared to numerical simulation and experimental results, showing a high agreement.

Delamination of kaolinite - potassium acetate intercalates by ball-milling

Structural changes in intercalated kaolinite after wet ball-milling were examined by scanning electron microscopy (SEM), X-ray diffraction (XRD), specific surface area (SSA) and Fourier Transform Infrared spectroscopy (FTIR). The X-ray diffraction pattern at room temperature indicated that the intercalation of potassium acetate into kaolinite causes an increase of the basal spacing from 0.718 to 1.42 nm, and with the particle size reduction, the surface area increased sharply with the intercalation and delamination by ball-milling. The wet ball-milling kaolinite after intercalation did not change the structural order, and the particulates have high aspect ratio according SEM images.

Synthesis and structural properties of Al-C-N-O composite thin films

Al-C-N-O composite thin films have been synthesized by radio frequency reactive diode sputtering of an aluminum target in plasmas of N2+O2+CH4 gas mixtures. The chemical structure and composition of the films have been investigated by means of infrared and X-ray photoelectron spectroscopy. The results reveal the formation of C-N, Al-C, Al-N and Al-O bonds. The X-ray diffraction pattern suggests that the films are of nanometer composite material and contain predominately crystalline grains of hexagonal AlN and α-Al2O3. A good thermal stability of the composite has been confirmed by the annealing treatment at temperatures up to 600 °C.

Polymer-mediated synthesis of γ-Fe2O3 nano-particles

Nano-particles of γ-Fe2O3 were synthesized by reacting polyethylene oxide–FeCl3 complex with NH4OH. These were characterized by X-ray diffraction (XRD), scanning electron miscroscopy (SEM), selected area electron diffraction (SAED) and transmision electron microscopy (TEM). The average particle size was found to be 10 nm, as determined from the line broadening of the main XRD peak. The crystalline phase was a spinel-type tetragonal structure, which was confirmed from the electron diffraction pattern. The zero field cooled magnetization of samples with varying γ-Fe2O3 content as a function of temperature was measured using a vibrating sample magnetometer. The magnetization curves show a peak at low temperature (15 K) corresponding to the blocking temperature TB. The value of TB was found to decrease with decreasing particle size. The magnetization measurements with respect to field at 5 and 170 K confirmed the transition from superparamagnetic to spin-glass state at TB, as evidenced from the remanence and hysteresis. These results can be explained on the basis of Néel's theory of superparamagnetism as applied to nano-particles.

Structural Transformations in Protein Crystals caused by controlled Dehydration

Recent experiments in this laboratory on structural transformations caused by controlled dehydration of protein crystals have been reviewed. X-ray diffraction patterns of the following crystals have been examined under varying conditions of environmental humidity in the relative humidity range of 100-75%: a new crystal form of bovine pancreatic ribonuclease A grown from acetone solution in tris buffer (I), the well-known monoclinic form of the protein grown from aqueous ethanol (II), the same form grown from a solution of 2-methyl pentan-2,4-diol in phosphate buffer (III), tetragonal (IV), orthorhombic (V), monoclinic (VI) and triclinic (VII) hen egg white lysozyme, porcine 2 Zn insulin (VIII), porcine 4 Zn insulin (IX) and the crystals of concanavalin A(X). I, II, IV, V and VI undergo one or more transformations as evidenced by discontinuous changes in the unit cell dimensions, the diffraction pattern and the solvent content. Such water-mediated transformations do not appear to occur in the remaining crystals in the relative humidity range explored. The relative humidity at which the transformation occurs is reduced when 2-methyl pentan-2,4-diol is present in the mother liquor. The transformations are affected by the crystal structure but not by the amount of solvent in the crystals. The X-ray investigations reviewed here and other related investigations emphasize the probable importance of water-mediated transformations in exploring hydration of proteins and conformational transitions in them.

Characterisation of sweetpotato from Papua New Guinea and Australia: Physicochemical, pasting and gelatinisation properties.

The physicochemical and functional properties of flours from 25 Papua New Guinean and Australian sweetpotato cultivars were evaluated. The cultivars (white-, orange-, cream-, and purple-fleshed, and with dry matter, from 15 to 28 g/100 g), were obovate, oblong, elliptic, curved, irregular in shape, and essentially thin-cortexed (1-2 mm). Flour yield was less than 90 g/100 g solids, while starch, protein, amylose, water absorption and solubility indices, as well as total sugars, varied significantly (p < 0.05). Potassium, sodium, calcium, and phosphorus were the major minerals measured, and there were differences in the pasting properties, which showed four classes of shear-thinning and shear-thickening behaviours. Differential scanning calorimetry showed single-stage gelatinisation behaviour, with cultivar-dependent temperatures (61-84 degrees C) and enthalpies (12-27 J/g dry starch). Oval-, round- and angular-shaped granules were observed with a scanning electron microscope, while X-ray diffraction revealed an A-type diffraction pattern in the cultivars, with about 30% crystallinity. This study shows a wide range of sweetpotato properties, reported for the first time.

Nd2O3 : Eu3+ nanocrystalline phosphor - a new potential thermoluminescing material for dosimetry

Nanoparticles of trivalent Eu3+-doped Nd2O3 phosphors have been prepared using a low-temperature solution combustion method with metal nitrate as precursor and oxalyldihydrazide as a fuel at a fairly low temperature (<500 degrees C) and in a very short time (<5 min). A powder X-ray diffraction pattern reveals that cubic Nd2O3 : Eu3+ crystallites are directly obtained without the requirement of further calcinations. The crystallite size, evaluated from Scherer's formula, was found to be in the range of 20-30 nm. The microstructure and morphology were studied by scanning electron microscopy, which showed the phosphor to be foamy and fluffy in nature. Thermoluminescence characteristics of the Nd2O3 : Eu3+ have been studied using gamma irradiation. These demonstrate that the phosphor is suitable for use as a dosimeter.

Phases in the (1-x)Na0.5Bi0.5TiO3-(x)CaTiO3 system

The structures of (1 - x) Na0.5Bi0.5TiO3-(x) CaTiO3 at room temperature have been investigated using neutron powder diffraction and dielectric studies. The system exhibits an orthorhombic (Pbnm) structure for x >= 0.15 and rhombohedral (R3c) for x <= 0.05. For x = 0.10, though the neutron diffraction pattern shows features of the orthorhombic (Pbnm) structure, Rietveld refinement using this structure shows a drastic reduction in the in-phase tilt angle (similar to 4 degrees) as compared to the corresponding value (similar to 8 degrees) for a neighbouring composition x = 0.15. The neutron diffraction pattern of x = 0.10 could be fitted equally well using a two-phase model (R3c + Pbnm) with orthorhombic as the minor phase (22%), without the need for a drastic decrease in the in-phase tilt angle. The dielectric studies of x = 0.10 revealed the presence of the polar R3c phase, thereby favouring the phase coexistence model, instead of a single-phase Pbnm structure, for this composition.

BCN:A Graphene Analogue with Remarkable Adsorptive Properties

A new analogue of graphene containing boron, carbon and nitrogen (BCN) has been obtained by the reaction of high-surface-area activated charcoal with a mixture of boric acid and urea at 900 degrees C. X-ray photoelectron spectroscopy and electron energy-loss spectroscopy reveal the composition to be close to BCN. The X-ray diffraction pattern, high-resolution electron microscopy images and Raman spectrum indicate the presence of graphite-type layers with low sheet-to-sheet registry. Atomic force microscopy reveals the sample to consist of two to three layers of BCN, as in a few-layer graphene. BCN exhibits more electrical resistivity than graphene, but weaker magnetic features. BCN exhibits a surface area of 2911 m(2)g(-1), which is the highest value known for a BxCyNz composition. It exhibits high propensity for adsorbing CO2 (approximate to 100 wt %) at 195 K and a hydrogen uptake of 2.6 wt % at 77 K. A first-principles pseudopotential-based DFT study shows the stable structure to consist of BN3 and NB3 motifs. The calculations also suggest the strongest CO2 adsorption to occur with a binding energy of 3.7 kJ mol(-1) compared with 2.0 kJ mol(-1) on graphene.