A hydride generation flow system for determination of arsenic and selenium by total reflection X-ray fluorescence spectrometry

In this work, a preconcentration and separation system based on continuous flow hydride generation is proposed to improve the determination of As and Se by total reflection X-ray fluorescence spectrometry. The generated hydrides are continuously separated from the liquid phase and collected in a chamber containing 250 mul of HCI/HNO3 1:1 (v/v) solution. Hydride generation conditions and collection of the hydrides were evaluated. Under optimised conditions, enrichment factors of 55 for As and 82 for Se were attained. Detection limits of 0.3 mug l(-1) for As and Se were obtained when 20 ml of sample was used. Analysis of a natural water standard reference material from National Institute of Standard and Technology (SRM-1640) was in agreement with the certified values at the 95% confidence level. (C) 2004 Elsevier B.V. All rights reserved.

Development and validation of an environmentally friendly attenuated total reflectance in the mid-infrared region method for the determination of ethanol content in used engine lubrication oil

Lubricating oils are crucial in the operation of automotive engines because they both reduce friction between moving parts and protect against corrosion. However, the performance of lubricant oil may be affected by contaminants, such as gasoline, diesel, ethanol, water and ethylene glycol. Although there are many standard methods and studies related to the quantification of contaminants in lubricant oil, such as gasoline and diesel oil, to the best of our knowledge, no methods have been reported for the quantification of ethanol in used Otto cycle engine lubrication oils. Therefore, this work aimed at the development and validation of a routine method based on partial least-squares multivariate analysis combined with attenuated total reflectance in the mid-infrared region to quantify ethanol content in used lubrication oil. The method was validated based on its figures of merit (using the net analyte signal) as follows: limit of detection (0.049%), limit of quantification (0.16%), accuracy (root mean square error of prediction=0.089% w/w), repeatability (0.05% w/w), fit (R 2 =0.9997), mean selectivity (0.047), sensitivity (0.011), inverse analytical sensitivity (0.016% w/w-1) and signal-to-noise ratio (max: 812.4 and min: 200.9). The results show that the proposed method can be routinely implemented for the quality control of lubricant oils. © 2013 Elsevier B.V. All rights reserved.

Monte Carlo simulation applied in total reflection X-ray fluorescence: Preliminary results

The X-ray Fluorescence (XRF) analysis is a technique for the qualitative and quantitative determination of chemical constituents in a sample. This method is based on detection of the characteristic radiation intensities emitted by the elements of the sample, when properly excited. A variant of this technique is the Total Reflection X-ray Fluorescence (TXRF) that utilizes electromagnetic radiation as excitation source. In total reflection of X-ray, the angle of refraction of the incident beam tends to zero and the refracted beam is tangent to the sample support interface. Thus, there is a minimum angle of incidence at which no refracted beam exists and all incident radiation undergoes total reflection. In this study, we evaluated the influence of the energy variation of the beam of incident x-rays, using the MCNPX code (Monte Carlo NParticle) based on Monte Carlo method. © 2013 AIP Publishing LLC.

Preparation and characterization of PVDF/CaCO3 composites

The contribution of new materials, involving composites and blends, has been reaching the most varied fields of science, as much of the scientific as technological point of view. This is due to the man's needs in applications, especially in medicine areas. Thus, this work shows the preparation and characterization of poly(vinylidene fluoride) (PVDF) and calcium carbonate (CaCO3) Composite films in order to analyse the incorporation of CaCO3 in PVDF for future application in bony restoration and bony filling. The films were prepared by casting method, where the PVDF pellet shape was dissolved in dimethylacetamide (DMA) and in a separate container CaCO3/DMA emulsion was also made. Soon afterwards they were mixed in several proportions 100/00, 95/05, 85/15, 70/30 in weight and left to dry in greenhouse. Homogeneous and flexible films were obtained and structurally characterized by attenuated total reflection infrared spectroscopy (FT-IR/ATR), thermal analyses (DSC, TGA), X-ray diffractometry, optical and scanning electron microscopies. The results showed that the material was a composite with good thermal stability until around 400 degrees C, the crystallinity of PVDF was non-polar alpha-phase and the obtained films were porous, being these filled with CaCO3. (c) 2006 Elsevier B.V. All rights reserved.

A micelle nucleation model for the interaction of dodecyl sulphate with Lys49-phospholipases A(2)

Bothropstoxin-I (BthTx-I) is a Lys49-PLA(2) from the venom of Bothrops jararacussu that lacks detectable catalytic activity, yet causes rapid Ca2+-independent membrane damage. With the aim of understanding the interaction between BthTx-I and amphiphilic molecules, we have studied the interaction of sodium dodecyl sulphate (SDS) with the protein. Circular dichroism and attenuated total reflection Fourier-transform infrared spectra of BthTx-I reveal changes in the alpha-helical organization of the protein at an SDS/BthTx-I molar ratio of 20-25. At SDS/BthTx-I ratios of 40-45 the alpha-helices return to a native-like conformation, although fluorescence emission anisotropy measurements of 2-amino-N-hexadecyl-benzamide (AHBA) demonstrate that the total SDS is below the critical micelle concentration when this transition occurs. These results may be interpreted as the result of SDS accumulation by the BthTx-I homodimer and the formation of a pre-micelle SDS/BthTx-I complex, which may subsequently be released from the protein surface as a free micelle. Similar changes in the alpha-helical organization of BthTx-I were observed in the presence of dipalmitoylphosphatidylcholine liposomes, suggesting that protein structure transitions coupled to organization changes of bound amphiphiles may play a role in the Ca2+-independent membrane damage by Lys49-PLA(2)s. (c) 2006 Elsevier B.V. All rights reserved.

Surface characterization of feldspathic ceramic using ATR FT-IR and ellipsometry after various silanization protocols

Objectives. This study characterized the feldspathic ceramic surfaces after various silanization protocols.Methods. Ceramic bars (2 mm x 4 mm x 10 mm) (N = 18) of feldpathic ceramic (VM7, VITA Zahnfabrik) were manufactured and finished. Before silane application, the specimens were ultrasonically cleaned in distilled water for 10 min. The ceramic specimens were randomly divided into nine groups (N = 2 per group) and were treated with different silane protocols. MPS silane (ESPE-Sil, 3M ESPE) was applied to all specimens and left to react at 20 degrees C for 2 min (G20). After drying, the specimens were subjected to heat treatment in an oven at 38 degrees C (G38), 79 degrees C (G79) or 100 degrees C (G100) for 1 min. Half of the specimens of each group were rinsed with water at 80 degrees C for 15 s (G20B, G38B, G79B, G100B). The control group (GC) received no silane. Attenuated total reflection infrared Fourier transform analysis (ATR FT-IR) was performed using a spectrometer. Thickness of silane layer was measured using a spectroscopic ellip-someter working in the lambda = 632.8 nm (He-Ne laser) at 70 degrees incidence angle. Surface roughness was evaluated using an optical profilometer. Specimens were further analyzed under the Scanning Electron Microscopy (SEM) to observe the topographic patterns.Results. ATR FT-IR analysis showed changes in Si-O peaks with enlarged bands around 940 cm(-1). Ellipsometry measurements showed that all post-heat treatment actions reduced the silane film thickness (30.8-33.5 nm) compared to G20 (40 nm). The groups submitted to rinsing in hot water (B groups) showed thinner silane films (9.8-14.4 nm) than those of their corresponding groups (without washing) (30.8-40 nm). Profilometer analysis showed that heat treatments (Ra approximate to 0.10-0.19 mu m; Rq approximate to 0.15-0.26 mu m) provided a smoother surface than the control group (Ra approximate to 0.48 mu m; Rq approximate to 0.65 mu m). Similar patterns were also observed in SEM images.Significance. Heat treatment after MPS silane application improved the silane layer network. Rinsing with boiling water eliminated the outmost unreacted regions of the silane yielding to thinner film thicknesses. (C) 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

A comparative study of the electrogeneration of hydrogen peroxide using Vulcan and Printex carbon supports

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Preparação e caracterização de tecidos tratados com polianilina condutora recobertos com borracha natural

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Adsorção-fotodegradação do herbicida paraquate em água pela argila Na-Bentonita e por novos materiais TiO2-Bentonita, TiO2/ZnOBentonita, Al/Fe-Bentonita e Al/Fe.Cu-Bentonita

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Análise multielementar da mucosa gástrica de roedores tratados com Alchornea glandulosa, Davilla elliptica e Davilla nitida pela técnica de fluorescência de raios-x por reflexão total

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Determinação da sensibilidade elementar de amostras-padrão pelo método de flurescência de raios X por reflexão total

To determinate the multielemental concentrations in biological samples using the technique of total reflection X-ray fluorescence (TRFX) is essential the use of standard samples. The aim of this study is the determination of the sensitivities of the relevant elements in standard samples (Multi Element atomic spectroscopy standard solution in HNO3 I) prepared in three solutions with different and known concentrations. Based on the sensitivities of the elements contained in the multilelementar standard sample, it can estimate the sensitivity for an element found in the biological sample and consequently it is possible to determinate the concentration, even though the standard does not contain this element. The measurement of fluorescence was performed at the Brazilian Synchrotron Light Laboratory (LNLS) in Campinas

Viabilidade do Código MCNPX para o Estudo da Técnica de Fluorescência de Raios-X por Reflexão Total

The X-ray fluorescence analysis (XRF) is an important technique for the qualitative and quantitative determination of chemical components in a sample. It is based on measurement of the intensity of the emitted characteristic radiation by the elements of the sample, after being properly excited. One of the modalities of this technique is the total reflection x-ray fluorescence (TXRF). In TXRF, the angle of refraction of the incident beam tends to zero and the refracted beam is tangent to the sample-support interface. Thus, there is a minimum angle of incidence that there is no refracted beam and all the incident radiation undergoes total reflection. As it is implemented in very small samples, in a film format, self-absorption effects should not very relevant. In this study, we evaluated the feasibility of using code MCNPX (Monte Carlo N - Particle eXtended), to simulate a measure implemented by the TXRF technique. In this way, it was verified the quality of response of a system by TXRF spectroscopy using synchrotron radiation as excitation beam for a simple setup, by retrieving the characteristic energies and the concentrations of the elements in the sample. The steps of data processing, after obtaining the excitation spectra, were the same as in a real experiment and included the obtaining of the sensitivity curve for the simulated system. The agreement between the theoretical and simulated values of Ka characteristic energies for different elements was lower than 1 % .The obtained concentration of the elements of the sample had high relatively errors ( between 6 and 60 % ) due mainly to lack of knowing about some realistic physical parameters of the sample , such as density . In this way, this result does not preclude the use of MCNPX code for this type of application

Exothermic Behavior, Degree of Conversion, and Viscoelastic Properties of Experimental and Commercially Available Hard Chairside Reline Resins

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Synergistic effect in the catalytic activity of lipase Rhizomucor miehei immobilized on zeolites for the production of biodiesel

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

The interaction between heparin and Lys49 phospholipase A(2) reveals the natural binding of heparin on the enzyme

We have studied at a molecular level the interaction of heparins on bothropstoxin-1 (BthTx-1), a phospholipase A(2) toxin. The protein was monitored using gel filtration chromatography, dynamic light scattering (DLS), circular dichroism (CD), attenuated total reflectance Fourier transform infrared (ATR-FTIR) and intrinsic tryptophan fluorescence emission (ITFE) spectroscopy. The elution profile of the protein presents a displacement of the protein peak to larger complexes when interacting with higher concentration of heparin. The DLS results shows two R-h at a molar ratio of 1, one to the distribution of the protein and the second for the action of heparin on BthTx-I structures, and a large distribution with the increase of protein. The interaction is accompanied by significant changes in the CD spectra, showing two common features: a decrease in signal at 208 nm (3 and 6 kDa heparins) and an isodichroic point near 226 nm (3 kDa heparin). FTIR spectra indicate that only a few amino acid residues are involved in this interaction. Alterations in the ITFE by binding heparins suggest that the initial binding occurs on the ventral face of BthTx-1. Together, these results add an experimental and structural basis on the action mechanism of the heparins over the phospholipases A(2) and provide a molecular model to elucidate the interaction of the enzyme-heparin complex at a molecular level. (c) 2005 Elsevier B.V. All rights reserved.