Crystallization of Arthrobacter sp. strain 1C N-(1-D-carboxyethyl)-L-norvaline dehydrogenase and its complex with NAD+

The novel NAD+-linked opine dehydrogenase from a soil isolate Arthrobacter sp. strain 1C belongs to an enzyme superfamily whose members exhibit quite diverse substrate specificites. Crystals of this opine dehydrogenase, obtained in the presence or absence of co-factor and substrates, have been shown to diffract to beyond 1.8 ? resolution. X-ray precession photographs have established that the crystals belong to space group P21212, with cell parameters a = 104.9, b = 80.0, c = 45.5 ? and a single subunit in the asymmetric unit. The elucidation of the three-dimensional structure of this enzyme will provide a structural framework for this novel class of dehydrogenases to enable a comparison to be made with other enzyme families and also as the basis for mutagenesis experiments directed towards the production of natural and synthetic opine-type compounds containing two chiral centres.     

Quantitation and characterization of phospholipids in pharmaceutical formulations by liquid chromatography-mass spectrometry

A simple and fast method for phospholipid analysis was developed using high-performance liquid chromatography-mass spectrometry with an atmospheric pressure ionization interface. Separation of the phospholipid molecular species was achieved using a linear gradient of a mixture of chloroform-10 mM ammonium acetate-methanol (30:5:65) on a silica column. Optimization of the mass spectrometer conditions has allowed the method to separate and detect the phospholipids mainly as protonated molecular species. In comparison to existing LC-MS methods, improvement in the total analysis time and sensitivity were achieved. Separation of all major phospholipid molecular classes was achieved in less than 6 min. Marked improvement was observed in the linearity of the response of the phospholipids studied providing a linear response over three orders of magnitude. Data supporting the validation of this method for the characterization of major phospholipids molecular species are also presented.     

Investigation of HfO(+) interference in the determination of platinum in a catalytic converter (cordierite) by inductively coupled plasma mass spectrometry

The determination of Pt in cordierite is subject to strong interference by spectral overlap from HfO(+) ions with all Pt isotopes. Two mathematical correction methods based on the HfO(+)Hf(+) ratio and a method for the chemical separation of Hf based on adsorption chromatography and isotope dilution were investigated to correct for this interference. Flow infection was used to prevent clogging of the cone orifice. To enhance the sensitivity and thus lower the detection limit, thermospray nebulization was used for sample introduction and the method was compared with pneumatic nebulization. In addition, the memory effects were evaulated for both systems. Analysis of artificial solutions (1 ng Pt ml(-1)) yielded results within 3% of the true value. Th Pt content (ca. 50 ng g(-1)) of a cordierite sample, previously exposed to exhaust gases, could be determined with precisions of about 10-25% and the results agreed with earlier determinations by other workers.     

Study of the electronic structure of rhenium and tungsten oxides on the O K-edge

Oxygen K-edge x-ray absorption spectra were studied on the electrochromic amorphous thin film a-WO₃ in the comparison with crystalline oxides having variable electronic (d⁰, d¹, d²) and atomic structure: monoclinic m-WO₃ (insulator - d⁰), cubic Na_0.6WO₃ (metal - d¹), cubic ReO₃ (metal - d¹), layered-type hexagonal h-WO₃, WO₃H₂O and with intercalated H_xReO₃ (metal - d²), H_xWO₃ oxides having a metal-isulating transition. The changes in the XANES range 10–15 eV above the absorption edge are interpreted based on the known band-structure calculations. The high-energy features are related to the multiple-scattering processes (EXAFS) on the nearest atoms. The intensity of the feature at 550–560 eV is attributed for the first time to the value of the metal-oxygen-metal bond angle. Paper presented at the 5th Euroconference on Solid State Ionics, Benalmádena, Spain, Sept. 13–20, 1998.     

Homotopy localization functorL f with respect to mapsf having a wedge of spheres as homotopy cofibre

In the connected case, we compute explicity thef-localization (in the sense of [3]) for the class of mapsZ ⁽ⁿ⁾↪Z in which the cofibre is a wedge of spheres. We have an analogous result over the rationals where the cofibre is arbitrary.     

Realization of single-mode telluride rib waveguides for mid-IR applications between 10 and 20 μm

The feasibility of all-telluride integrated optics devices based on waveguides presenting a single-mode behavior in the spectral range (10-20 μm) is demonstrated. These waveguides are constituted of a several micrometer thick Te(82)Ge(18) film deposited onto a Te(75)Ge(15)Ga(10) bulk glass substrate by thermal coevaporation and further etched by reactive ion etching under the CHF(3)/O(2)/Ar atmosphere. The obtained structures were proven to behave as channel waveguides with a good single-mode transmission over the whole spectral range. These results allowed validating our technological solution for the fabrication of integrated optics modal filters for spatial interferometry.     

Influence of surfactant structure on reverse micelle size and charge for nonpolar electrophoretic inks

Electrophoretic inks, which are suspensions of colorant particles that are controllably concentrated and dispersed by applied electric fields, are the leading commercial technology for high-quality reflective displays. Extending the state of the art for high-fidelity color in these displays requires improved understanding and control of the colloidal systems. In these inks, reverse micelles in nonpolar media play key roles in media and particle charging. Here we investigate the effect of surfactant structure on reverse micelle size and charging properties by synthesizing different surfactants with variations in polyamine polar head groups. Small-angle X-ray scattering (SAXS) and dynamic light scattering (DLS) were used to determine the micelle core plus shell size and micelle hydrodynamic radius, respectively. The results from SAXS agreed with DLS and showed that increasing polyamines in the surfactant head increased the micelle size. The hydrodynamic radius was also calculated on the basis of transient current measurements and agreed well with the DLS results. The transient current technique further determined that increasing polyamines increased the charge stabilization capability of the micelles and that an analogous commercial surfactant OLOA 11000 made for a lower concentration of charge-generating ions in solution. Formulating magenta inks with the various surfactants showed that the absence of amine in the surfactant head was detrimental to particle stabilization and device performance.     

Thermal analyses of organic powders made from precipitation polymerization of triallyl monomers

Organic solids have been prepared from radical-initiated activation of solutions composed of tetradecane and triallyl trimesate (TAM) monomer or triallyl phosphate (TAP) monomer using a recently developed variation of precipitation polymerization methods. The powders, which comprise fused aggregates, are shown to be rich in monomer (83–88 wt% TAM or 86–92 wt% TAP), and are believed to be formed by a combination of hydrocarbon addition and allyl group oligomerization. TAM-g-tetradecane primary particles are on the order of 500 nm in diameter, while TAP-g-tetradecane particles are on the order of 100–200 nm diameter. These products are thermochemically assessed using a combination of differential scanning calorimetry, thermogravimetry and pyrolysis combustion flow calorimetry. The phosphorus-containing TAP-g-tetradecane shows exothermic activity around 230 °C, likely due to thermal decomposition of the trialkyl phosphate moiety, and may find use in advanced materials applications.