Nucleation and crystallization of titania nanoparticles in silica titania planar waveguides: A study by low frequency Raman scattering

SiO2 (1-x) - TiO2 (x) waveguides, with the mole fraction x in the range 0.07 - 0.20 and thickness of about 0.4 μm, were deposited on silica substrates by a dip-coating technique. The thermal treatments at 700-900°C, used to fully densify the xerogels, produce nucleation of TiO2 nanocrystals even for the lowest TiO2 content. The nucleation of TiO2 nanocrystals and their growth by thermal annealing up to 1300°C were studied by waveguide Raman spectroscopy, for the SiO2 (0.8) - TiO2 (0.2) composition. By increasing the annealing temperature, the Raman spectrum evolves from that typical of the silica-titania glass to that of anatase, but brookite phase is dominant at intermediate temperatures. In the low. frequency region (5-50 cm-1) of the Raman spectra, acoustic vibrations of the nanocrystals are observed. From the measured line shapes, we can deduce the size distribution of the particles. The results are compared with those obtained from the line widths in the X-ray diffraction patterns. Nanocrystals with a mean size in the range 4-20 nm are obtained, by thermal annealing in a corresponding range of 800-1300°C.

Determination of methyldopa in pharmaceutical formulations by combined spot test-diffuse reflectance spectroscopy

This paper describes a very simple and rapid quantitative reflectance spot test procedure for the determination of methyldopa in pharmaceutical formulations. This method is based on the complexation reaction of methyldopa with molybdate ions yielding a yellow stable complex on filter paper. Reflectance measurements were carried out at 410 nm. Under optimal conditions, the calibration graphs obtained for methyldopa by plotting the optical density of the reflectance signal (A R) vs. the log of the concentration were linear from 6.30 × 10 -3 to 1.89 × 10 -2 mol L -1, with a correlation coefficient of 0.998. The detection limit was 2.74 × 10 -3 mol L -1 (R.S.D. = 1.02%) for methyldopa. The common excipients used as additives in pharmaceuticals do not interfere in the proposed method. The method was applied to determine metyldopa in commercial pharmaceutical formulations. The results obtained by the proposed method compare favorably with those obtained by an official procedure at 95% confidence level. ©2006 Sociedade Brasileira de Química.

Charmed-meson scattering on nucleons in a QCD Coulomb gauge quark model

The scattering of charmed mesons on nucleons is investigated within a chiral quark model inspired on the QCD Hamiltonian in Coulomb gauge. The microscopic model incorporates a longitudinal Coulomb confining interaction derived from a self-consistent quasi-particle approximation to the QCD vacuum, and a traverse hyperfine interaction motivated from lattice simulations of QCD in Coulomb gauge. From the microscopic interactions at the quark level, effective meson-baryon interactions are derived using a mapping formalism that leads to quark-Born diagrams. As an application, the total cross-section of heavy-light D-mesons scattering on nucleons is estimated.

Determination of atenolol in pharmaceutical formulations by diffuse reflectance spectroscopy

A simple analytical method for quantification of atenolol in pharmaceutical formulations by diffuse reflectance spectroscopy is described. The method is based on the reaction, on the filter paper surface, between the drug and p-chloranil producing a colored compound. The best reaction conditions were obtained with 20 μL of atenolol solution and 20 μL of p-chloranil. All reflectance measurements were carried out at 550 nm and the linear range was from 1.13×10-2 to 7.88×10-2 mol L-1 (r = 0.9992). The limit of detection was 2.80 × 10-3 mol L-1. The proposed method was successfully applied to analysis of different commercial brands of pharmaceutical formulations and the results obtained by the proposed method were in good agreement with those obtained using the British Pharmacopoeia method.

Diffuse Effect of the Tungsten Doped Ba(Zr0.10Ti0.90)O3 Ferroelectric Ceramics

Barium zirconate titanate Ba(Ti0.90Zr0.10)O3 ceramics doped with WO3 (BZT:2W) have been prepared by a traditional solid phase reaction. The effect of temperature on the structural and electrical properties was investigated. X ray diffraction data evidenced formation of secondary phases for the samples sintered at 1300oC end 1350oC while the pure phase was attained at 1200oC. A modified Curie-Weiss law was used to describe the diffuseness of a phase transition. As temperature increases, the maximum dielectric permittivity decreased. The fine-grained sample showed a 'diffuse-like' ferroelectric behavior. The dielectric permittivity reaches a maximum value (εm ~6420 at 10 kHz) for the ceramics sintered at 1200oC for 4 hours.

Heavy-light mesons scattering from nucleons: Quark-gluon and meson exchanges

We investigate the scattering of heavy-light K and D mesons by nucleons at low energies. The short-distance part of the interaction is described by quark-gluon interchange and the longdistance part is described by a one-meson-exchange model that includes the contributions of vector (ρ, ω) and scalar (σ) mesons. The microscopic quark model incorporates a confining Coulomb potential extracted from lattice QCD simulations and a transverse hyperfine interaction consistent with a finite gluon propagator in the infrared. The derived effective meson-nucleon potential is used in a Lippmann-Schwinger equation to obtain s-wave phase shifts. Our final aim is to set up a theoretical framework that can be extended to finite temperatures and baryon densities. © 2010 American Institute of Physics.

Annual and monthly mean global, direct and diffuse solar irradiation in Botucatu/SP/Brazil

This paper presents a climatic and statistical analysis of global, direct horizontal and diffuse radiation from a database of solar radiation measured from 1996 to 2006 in the city of Botucatu, SP, Brazil. Variation intervals of hourly and daily irradiation, annual mean 〈H̄G〉, 〈H̄bh〉 and 〈H̄d〉 irradiation, monthly mean 〈H̄G〉, 〈H̄ bh〉 and 〈H̄d〉 irradiation and monthly mean 〈K̄t〉, 〈K̄bh〉 and 〈K̄d〉 fractions were determined. Results showed that values of hourly and daily annual mean irradiation were as follows: 〈H̄G〉=1.49MJ/m2 and 〈H̄ G〉=17.74MJ/m2; 〈H̄bh〉=0. 90MJ/m2 and 〈H̄bh〉=10.33MJ/m2 and 〈H̄d〉=0.57 MJ/m2 and 〈H̄d〉=7.09MJ/m2, respectively. Variation intervals of hourly monthly mean irradiation were as follows: 〈H̄G〉 ranged from 1.65MJ/m2 in March to 1.16MJ/m2 in June; 〈H̄bh〉 ranged from 1.06MJ/m2 in April to 0.79MJ/m2 in June, and 〈H̄d〉 ranged from 0.70MJ/m2 in January to 0.37MJ/m2 in June and July. Similarly, daily 〈H̄ G〉 irradiation ranged from 21.35MJ/m2 in November to 12.94MJ/m2 in June; 〈H̄bh〉 ranged from 11.83MJ/m2 in April to 8.49MJ/m2 in June, and 〈H̄d〉 ranged from 10.29MJ/m2 in December to 4.38MJ/m2 in June. Variation intervals of hourly monthly mean fractions were as follows: 〈K̄t〉 ranged from 43.5% in January to 54.2% in April; 〈K̄bh〉 ranged from 33.6% in January to 58.0% in April and 〈K̄d〉 ranged from 66.4% in January to 42.0% in April. In the same way, daily 〈K̄ t〉 fractions ranged from 45.5% in January to 59.8% in August; 〈K̄bh〉 ranged from 38.9% in January to 62.0% in August and 〈K̄d〉 ranged from 61.1% in January to 37.7% in July.

Numerical correction for the diffuse solar irradiance by the melo-escobedo shadowring measuring method

The present paper deals with numerical corrections factors proposed as a function of the clearness index in order to correct the diffuse solar irradiance measured with the Melo-Escobedo Shadowring Measuring Method (ME shadowring). The global irradiance was measured by an Eppley - PSP pyranometer ; direct normal irradiance by an Eppley-NIP pyrheliometer fitted to a ST-3 sun tracking device and the diffuse irradiance by an Eppley-PSP pyranometer fitted to a ME shadowring. The validations were performed by the MBE and RMSE statistical indicators. The results showed that the numerical correction factors were appropriate to correct the shadowring diffuse irradiance.

Surface-enhanced Raman scattering (SERS) applied to cancer diagnosis and detection of pesticides, explosives, and drugs

The inelastic scattering of light, Raman scattering, presents a very low cross section. However, the signal can be amplified by several orders of magnitude, leading to the so-called surface-enhanced Raman scattering (SERS) phenomenon. Basically, the SERS effect is achieved when the target molecule (analyte) is adsorbed onto metallic nanoparticles, usually noble metals. This article presents an overview of the applications of SERS to cancer diagnosis and the detection of pesticides, explosives, and drugs (illicit and pharmacological). SERS is routinely applied nowadays to detect and identify analytes at very low concentrations, including for single-molecule detection. However, the application of SERS as an analytical tool requires reliable and reproducible SERS substrates, in terms of enhancement factors, which depends on the size, shape, and aggregation of the metallic nanoparticles. Therefore, the production of reliable and reproducible SERS substrates is a challenge in the field. Besides, the metallic nanoparticles can also induce changes in the system by possible interactions with the analyte under investigation, which must be taken into account. This review will present work in which, under certain specific experimental conditions, SERS has been analytically applied.

Rapid determination of furosemide by combined spot test/diffuse reflectance spectroscopy to detect doping in sport

This paper describes the development and application of a simple, cheap, and clean method for the quantification of furosemide in urine samples from athletes, to detect doping, using a combined spot test/diffuse reflectance spectroscopy procedure. The method is based on the complexation reaction of furosemide (5-(aminosulfonyl)-4-chloro-2-((furanylmethyl)amino)benzoic acid, dissolved in ethanol, with FeCl3 and the surfactant dodecyltrimethylammonium bromide (DTAB) in aqueous solution, yielding a colored compound on the surface of a filter paper. The reagent concentrations were optimized using a chemometric experimental design. The reflectometric measurements of the complex formed were carried out at 477nm. The linear range obtained was 1.65-9.00×10-3molL-1 of furosemide (R=0.997), and the detection and quantification limits were 4.9×10-4 and 1.62×10-3molL-1, respectively. The proposed method was successfully applied in the analysis of furosemide in spiked urine, demonstrating that it is a reliable alternative method for the detection of furosemide doping in sport. © 2012 Elsevier B.V..

Small-angle X-ray scattering and structural modeling of full-length: Cellobiohydrolase I from Trichoderma harzianum

Cellobiohydrolases hydrolyze cellulose releasing cellobiose units. They are very important for a number of biotechnological applications, such as, for example, production of cellulosic ethanol and cotton fiber processing. The Trichoderma cellobiohydrolase I (CBH1 or Cel7A) is an industrially important exocellulase. It exhibits a typical two domain architecture, with a small C-terminal cellulose-binding domain and a large N-terminal catalytic core domain, connected by an O-glycosylated linker peptide. The mechanism by which the linker mediates the concerted action of the two domains remains a conundrum. Here, we probe the protein shape and domain organization of the CBH1 of Trichoderma harzianum (ThCel7A) by small angle X-ray scattering (SAXS) and structural modeling. Our SAXS data shows that ThCel7A linker is partially-extended in solution. Structural modeling suggests that this linker conformation is stabilized by inter- and intra-molecular interactions involving the linker peptide and its O-glycosylations. © 2013 Springer Science+Business Media Dordrecht.

Estimates of hourly diffuse radiation on tilted surfaces in southeast of brazil

The global radiation incident on a tilted surfaces consists of components direct, diffuse and reflected from the ground. On a hourly database, the direct radiation can be calculated by geometric projections (ratio of the incidence angle to the solar zenith angle). The reflected radiation has a small effect on calculations and may be calculated with an isotropic model. Both components presents dependence of measures in incidence or horizontal surface. The great difficulty is to evaluate the diffuse radiation by variations of circumsolar, brightness horizontal, isotropic and anisotropic subcomponents. This study evaluated twenty models to estimate hourly diffuse radiation incident on tilted surfaces at 12.85° (latitude - 10°), 22.85° (latitude) and 32.85° (latitude + 10°) facing to North, under different cloudiness sky conditions, in Botucatu, São Paulo State, Brazil (22°53' S, 48°26' W and 786 m above the mean sea level). In contrast, models for estimating the diffuse component show major differences, which justify the validation for local calibrations. There is a decrease of the maximum total radiation scattered with increasing atmospheric transmissivity and inclination angle. The best results are obtained by anisotropic models: Ma and Iqbal, Hay, Reindl et al. and Willmott; isotropic: Badescu and Koronakis, and the Circumsolar model. The increase of the inclination angle allows for a reduction in the performance of statistical parametric models for estimating the hourly diffuse radiation.

Estimativas das radiações direta e difusa em superfícies inclinadas com base na razáo de insolação

Statistical equations were obtained and evaluated with annual, seasonal and monthly data groupings for estimates of direct and diffuse components of solar radiation based on the sunshine duration (ratio of sunshine and photoperiod) incident on horizontal and inclined surfaces to 12.85, 22.85 and 32.85° with facing to North, in Botucatu, SP. The ratios between the two components and radiation at the top of the atmosphere were used, in a database whose inclinations were measured in three different periods (22.85°: 04/1998 to 07/2001; 12.85°: 08/2011 to 02/2003; and 32.85°: 03/2003 to 12/2007) and concomitant with horizontal measures and sunshine duration. The correlations showed a linear and second degree polynomial behavior for the direct and diffuse radiation, with higher coefficients of determination in periods of low variation in the coverage of the sky (cloudiness). The highest values of the direct and diffuse radiation were found in winter and summer, respectively for all surfaces evaluated. The increase in the inclination angle decreased the performance of equations in all groups of data with increase in scattering and decrease in index of the adjustment, however, the monthly equations allowed better performance for the two components.

Sodium dodecyl sulfate (SDS) effect on the thermal stability of oxy-HbGp: Dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) studies

Glossoscolex paulistus (HbGp) hemoglobin is an oligomeric protein, presenting a quaternary structure constituted by 144 globin and 36 non-globin chains (named linkers) with a total molecular mass of 3.6MDa. SDS effects on the oxy-HbGp thermal stability were studied, by DLS and SAXS, at pH 5.0, 7.0 and 9.0. DLS and SAXS data show that the SDS-oxy-HbGp interactions induce a significant decrease of the protein thermal stability, with the formation of larger aggregates, at pH 5.0. At pH 7.0, oxy-HbGp undergoes complete oligomeric dissociation, with increase of temperature, in the presence of SDS. Besides, oxy-HbGp 3.0mg/mL, pH 7.0, in the presence of SDS, has the oligomeric dissociation process reduced as compared to 0.5mg/mL of protein. At pH 9.0, oxy-HbGp starts to dissociate at 20°C, and the protein is totally dissociated at 50°C. The thermal dissociation kinetic data show that oxy-HbGp oligomeric dissociation at pH 7.0, in the presence of SDS, is strongly dependent on the protein concentration. At 0.5mg/mL of protein, the oligomeric dissociation is complete and fast at 40 and 42°C, with kinetic constants of (2.1±0.2)×10-4 and (5.5±0.4)×10-4s-1, respectively, at 0.6mmol/L SDS. However, at 3.0mg/mL, the oligomeric dissociation process starts at 46°C, and only partial dissociation, accompanied by aggregates formation is observed. Moreover, our data show, for the first time, that, for 3.0mg/mL of protein, the oligomeric dissociation, denaturation and aggregation phenomena occur simultaneously, in the presence of SDS. Our present results on the surfactant-HbGp interactions and the protein thermal unfolding process correspond to a step forward in the understanding of SDS effects. © 2013 Elsevier B.V.

Análise da região do anel F de Saturno

Pós-graduação em Física - FEG