Short-range structure of Pb(1-x)Ba(x)Zr(0.65)Ti(0.35)O(3) ceramic compounds probed by XAS and Raman scattering techniques

Ti K-edge x-ray absorption near-edge spectroscopy (XANES) and Raman scattering were used to study the solid solution effects on the structural and vibrational properties of Pb(1-x)Ba(x)Zr(0.65)Ti(0.35)O(3) with 0.0 < x < 0.40. Compared with x-ray diffraction techniques, which indicates that the average crystal symmetry changes with the substitution of Pb by Ba ions or with temperature variations for samples with x=0.00, 0.10, and 0.20, local structural probes such as XANES and Raman scattering results demonstrate that at local level, the symmetry changes are much less prominent. Theoretical XANES spectra calculation corroborate with the interpretation of the XANES experimental data.

Structure and magnetism of homometallic ludwigites: Co(3)O(2)BO(3) versus Fe(3)O(2)BO(3)

We present an extensive study of the structural, magnetic, and thermodynamic properties of the oxyborate Co(3)O(2)BO(3). This is carried out through x-ray diffraction, static and dynamic magnetic susceptibilities, and specific heat experiments in single crystals in a large temperature range. The structure of Co(3)O(2)BO(3) is composed of subunits in the form of three-leg ladders where Co ions with mixed valency are located. The magnetic properties of this Co ludwigite are determined by a competition between superexchange and double-exchange interactions in the low-dimensional subunits. We discuss the observed physical properties in comparison with the only other known homometallic ludwigite, Fe(3)O(2)BO(3). The latter presents a structural distortion in the ladders and two magnetic transitions. Both features are not found in the present study of the Co ludwigite. The reason for these differences in the structural and magnetic behavior of two apparently similar compounds is discussed.

Thermal lens and heat generation of Nd : YAG lasers operating at 1.064 and 1.34 mu m

We report on a simple and accurate method for determination of thermo-optical and spectroscopic parameters (thermal diffusivity, temperature coefficient of the optical path length change, pump and fluorescence quantum efficiencies, thermal loading, thermal lens focal length, etc) of relevance in the thermal lensing of end-pumped neodymium lasers operating at 1.06- and 1.3-mu m channels. The comparison between thermal lensing observed in presence and absence of laser oscillation has been used to elucidate and evaluate the contribution of quantum efficiency and excited sate absorption processes to the thermal loading of Nd: YAG lasers. (c) 2008 Optical Society of America.

Thermo-optical characteristics and concentration quenching effects in Nd(3+)doped yttrium calcium borate glasses

In this work we present a comprehensive study of the spectroscopic and thermo-optical properties of a set of samples with composition xNd(2)O(3)-(5-x)Y(2)O(3-)40CaO-55B(2)O(3) (0 <= x <= 1.0 mol%). Their fluorescence quantum efficiency (eta) values were determined using the thermal lens technique and the dependence on the ionic concentration was analyzed in terms of energy transfer processes, based on the Forster-Dexter model of multipolar ion-ion interactions. A maximum eta = 0.54 was found to be substantially higher than for yttrium aluminoborate crystals and glasses with comparable Nd(3+) content. As for the thermo-optical properties of yttrium calcium borate, they are comparable to other well-known laser glasses. The obtained energy transfer microparameters and the weak dependence of. on the Nd(3+) concentration with a high optimum Nd(3+) concentration put this system as a strong candidate for photonics applications. (C) 2011 American Institute of Physics. [doi:10.1063/1.3567091]

Crystallization and preliminary X-ray diffraction analysis of a glutathione S-transferase from Xylella fastidiosa

Glutathione S-transferases (GSTs) form a group of multifunctional isoenzymes that catalyze the glutathione-dependent conjugation and reduction reactions involved in the cellular detoxification of xenobiotic and endobiotic compounds. GST from Xylella fastidiosa (xfGST) was overexpressed in Escherichia coli and purified by conventional affinity chromatography. In this study, the crystallization and preliminary X-ray analysis of xfGST is described. The purified protein was crystallized by the vapour-diffusion method, producing crystals that belonged to the triclinic space group P1. The unit-cell parameters were a = 47.73, b = 87.73, c = 90.74 angstrom, alpha = 63.45, beta = 80.66, gamma = 94.55 degrees. xfGST crystals diffracted to 2.23 angstrom resolution on a rotating-anode X-ray source.

Upconversion in Nd(3+)-doped glasses: Microscopic theory and spectroscopic measurements

In this work, we report a systematic investigation of upconversion losses and their effects on fluorescence quantum efficiency and fractional thermal loading in Nd(3+)-doped fluoride glasses. The energy transfer upconversion (gamma(up)) parameter, which describes upconversion losses, was experimentally determined using different methods: thermal lens (TL) technique and steady state luminescence (SSL) measurements. Additionally, the upconversion parameter was also obtained from energy transfer models and excited state absorption measurements. The results reveal that the microscopic treatment provided by the energy transfer models is similar to the macroscopic ones achieved from the TL and SSL measurements because similar gamma(up) parameters were obtained. Besides, the achieved results also point out the migration-assisted energy transfer according to diffusion-limited regime rather than hopping regime as responsible for the upconversion losses in Nd-doped glasses. (c) 2008 American Institute of Physics.

Crystallization and preliminary structural analysis of the giant haemoglobin from Glossoscolex paulistus at 3.2 angstrom

Glossoscolex paulistus is a free-living earthworm encountered in south-east Brazil. Its oxygen transport requirements are undertaken by a giant extracellular haemoglobin, or erythrocruorin (HbGp), which has an approximate molecular mass of 3.6 MDa and, by analogy with its homologue from Lumbricus terrestris (HbLt), is believed to be composed of a total of 180 polypeptide chains. In the present work the full 3.6 MDa particle in its cyanomet state was purified and crystallized using sodium citrate or PEG8000 as precipitant. The crystals contain one-quarter of the full particle in the asymmetric unit of the I222 cell and have parameters of a = 270.8 angstrom, b = 320.3 angstrom and c = 332.4 angstrom. Diffraction data were collected to 3.15 angstrom using synchrotron radiation on beamline X29A at the Brookhaven National Laboratory and represent the highest resolution data described to date for similar erythrocruorins. The structure was solved by molecular replacement using a search model corresponding to one-twelfth of its homologue from HbLt. This revealed that HbGp belongs to the type I class of erythrocruorins and provided an interpretable initial electron density map in which many features including the haem groups and disulfide bonds could be identified.

Development and validation of a fast RP-HPLC method to determine the analogue of the thyroid hormone, 3,5,3 '-triiodothyroacetic acid (TRIAC), in polymeric nanoparticles

The objective of this work was to develop and validate a rapid Reversed-Phase High-Performance Liquid Chromatography method for the quantification of 3,5,3 '-triiodothyroacetic acid (TRIAC) in nanoparticles delivery system prepared in different polymeric matrices. Special attention was given to developing a reliable reproductive technique for the pretreatment of the samples. Chromatographic runs were performed on an Agilent 1200 Series HPLC with a RP Phenomenex (R) Gemini C18 (150 x 4, 6 mm i.d., 5 mu m) column using acetonitrile and triethylamine buffer 0.1% (TEA) (40 : 60 v/v) as a mobile phase in an isocratic elution, pH 5.6 at a flow rate of 1 ml min(-1). TRIAC was detected at a wavelength of 220 nm. The injection volume was 20 mu l and the column temperature was maintained at 35 degrees C. The validation characteristics included accuracy, precision, specificity, linearity, recovery, and robustness. The standard curve was found to have a linear relationship (r(2) - 0.9996) over the analytical range of 5-100 mu g ml(-1) . The detection and quantitation limits were 1.3 and 3.8 mu g ml(-1), respectively. The recovery and loaded TRIAC in colloidal system delivery was nearly 100% and 98%, respectively. The method was successfully applied in polycaprolactone, polyhydroxybutyrate, and polymethylmethacrylate nanoparticles.

Purification, crystallization and preliminary crystallographic analysis of the catalytic domain of the extracellular cellulase CBHI from Trichoderma harzianum

The filamentous fungus Trichoderma harzianum has a considerable cellulolytic activity that is mediated by a complex of enzymes which are essential for the hydrolysis of microcrystalline cellulose. These enzymes were produced by the induction of T. harzianum with microcrystalline cellulose (Avicel) under submerged fermentation in a bioreactor. The catalytic core domain (CCD) of cellobiohydrolase I (CBHI) was purified from the extracellular extracts and submitted to robotic crystallization. Diffraction-quality CBHI CCD crystals were grown and an X-ray diffraction data set was collected under cryogenic conditions using a synchrotron-radiation source.

The role of quantum confinement and crystalline structure on excitonic lifetimes in silicon nanoclusters

The emission energy dependence of the photoluminescence (PL) decay rate at room temperature has been studied in Si nanoclusters (Si-ncl) embedded in Si oxide matrices obtained by thermal annealing of substoichiometric Si oxide layers Si(y)O(1-y), y=(0.36,0.39,0.42), at various annealing temperatures (T(a)) and gas atmospheres. Raman scattering measurements give evidence for the formation of amorphous Si-ncl at T(a)=900 degrees C and of crystalline Si-ncl for T(a)=1000 degrees C and 1100 degrees C. For T(a)=1100 degrees C, the energy dispersion of the PL decay rate does not depend on sample fabrication conditions and follows previously reported behavior. For lower T(a), the rate becomes dependent on fabrication conditions and less energy dispersive. The effects are attributed to exciton localization and decoherence leading to the suppression of quantum confinement and the enhancement of nonradiative recombination in disordered and amorphous Si-ncl. (C) 2010 American Institute of Physics. [doi: 10.1063/1.3457900]

Protein preparation, crystallization and preliminary X-ray analysis of Trypanosoma cruzi nucleoside diphosphate kinase 1

The flagellated protozoan parasite Trypanosoma cruzi is the aetiological agent of Chagas disease. Nucleoside diphosphate kinases (NDPKs) are enzymes that are involved in energy management and nucleoside balance in the cell. T. cruzi TcNDPK1, a canonical isoform, was overexpressed in Escherichia coli as an N-terminally poly-His-tagged fusion protein and crystallized. Crystals grew after 72 h in 0.2 M MgCl(2), 20% PEG 3350. Data were collected to 3.5 angstrom resolution using synchrotron X-ray radiation at the National Synchrotron Light Laboratory (Campinas, Brazil). The crystals belonged to the trigonal space group P3, with unit-cell parameters a = b = 127.84, c = 275.49 angstrom. Structure determination is under way and will provide relevant information that may lead to the first step in rational drug design for the treatment of Chagas disease.

Luminescent and thermo-optical properties of Nd(3+)-doped yttrium aluminoborate laser glasses

In this work we performed a thorough spectroscopic and thermo-optical investigation of yttrium aluminoborate glasses doped with neodymium ions. A set of samples, prepared by the conventional melt-quenching technique and with Nd(2)O(3) concentrations varying from 0.1 to 0.75 mol %, were characterized by ground state absorption, photoluminescence, excited state lifetime measurements, and thermal lens technique. For the neodymium emission at 1064 nm ((4)F(3/2) -> (4)I(11/2) transition), no significant luminescence concentration quenching was observed and the experimental lifetime values ranged around 70 mu s. The obtained values of thermal conductivity and diffusivity of approximately 10.3 x 10(-3) W / cm K and 4.0 x 10(-3) cm(2) / s, respectively, are comparable to those of commercial laser glasses. Moreover, the fluorescence quantum efficiency of the glasses, calculated using the Judd-Ofelt formalism and luminescence decay, lies in the range from 0.28 to 0.32, larger than the typical values obtained for Nd(3+) doped YAl(3)(BO(3))(4) crystals. (c) 2009 American Institute of Physics. [DOI: 10.1063/1.3176503]

NMR quadrupolar system described as Bose-Einstein-condensate-like system

This paper presents a description of nuclear magnetic resonance (NMR) of quadrupolar systems using the Holstein-Primakoff (HP) formalism and its analogy with a Bose-Einstein condensate (BEC) system. Two nuclear spin systems constituted of quadrupolar nuclei I=3/2 ((23)Na) and I=7/2 ((133)Cs) in lyotropic liquid crystals were used for experimental demonstrations. Specifically, we derived the conditions necessary for accomplishing the analogy, executed the proper experiments, and compared with quantum mechanical prediction for a Bose system. The NMR description in the HP representation could be applied in the future as a workbench for BEC-like systems, where the statistical properties may be obtained using the intermediate statistic, first established by Gentile. The description can be applied for any quadrupolar systems, including new developed solid-state NMR GaAS nanodevices.

Partial magnetic ordering and crystal structure of the ludwigites Co(2)FeO(2)BO(3) and Ni(2)FeO(2)BO(3)

We present an extensive study of the structural, magnetic, and thermodynamic properties of the two heterometallic oxyborates: Co(2)FeO(2)BO(3) and Ni(2)FeO(2)BO(3). This has been carried out through x-ray diffraction at room temperature (RT) and 150 K, dc and ac magnetic susceptibilities, and specific-heat experiments in single crystals above 2 K. The magnetic properties of these iron ludwigites are discussed in comparison with those of the other two known homometallic ludwigites: Fe(3)O(2)BO(3) and Co(3)O(2)BO(3). In both ludwigites now studied we have found that the magnetic ordering of the Fe(3+) ions occurs at temperatures very near to which they order in Fe(3)O(2)BO(3). A freezing of the divalent ions (Co and Ni) is observed at lower temperatures. Our x-ray diffraction study of both ludwigites at RT and 150 K showed very small ionic disorder in apparent contrast with the freezing of the divalent ion spins. The structural transition that occurs in homometallic Fe(3)O(2)BO(3) has not been found in the present mixed ludwigites in the temperature range investigated.

Crystallization and preliminary X-ray diffraction analysis of human IL-22 bound to its soluble decoy receptor IL-22BP

Interleukin-22 (IL-22) is a pleiotropic cytokine that is involved in inflammatory responses. Human IL-22 was incubated with its soluble decoy receptor IL-22BP (IL-22 binding protein) and the IL-22 -IL-22BP complex was crystallized in hanging drops using the vapour-diffusion method. Suitable crystals were obtained from polyethylene glycol solutions and diffraction data were collected to 2.75 angstrom resolution. The crystal belonged to the tetragonal space group P41, with unit-cell parameters a = b = 67.9, c = 172.5 angstrom, and contained two IL-22-IL- 22BP complexes per asymmetric unit.