Ultra-thin films of alternating semi-interpenetrating layers of a conducting polymer with thermosetting phenolic resins for sensor application

In this work a new method for crosslinking ultra-thin films with potential applications in sensor systems is proposed. The films were produced by layer-by-layer (LbL) assembly using a conducting polymer, poly(o-ethoxyaniline) (POEA), alternated with a thermosetting resin, novolac-type phenolformaldehyde (PF), crosslinked by a simple thermal treatment. The PF resin served as both alternating and crosslinking agents. The films were characterized by Fourier transform infrared (FTIR) and ultraviolet-visible (UV-Vis) spectroscopy, thermogravimetry (TG), desorption, doping/dedoping cycling and electrical measurements. The results showed that film architecture and crosslinking degree can be controlled by the conditions used for film deposition (number of bilayers, polymer concentration, pH, and deposition time), and crosslinking time. Moreover, this approach offers several advantages such as fast curing time and low cost, indicating that these films can be used to produce sensors with improved stability.

Synthesis and characterization of semiconductor polymers having different phenylene-vinylene conjugation lengths

We have synthesized phenylene-vinylene (PV) polymers containing segments with different conjugation lengths interspaced by random distributed aliphatic segments. Infrared (IR) and ultraviolet-visible (UV-vis) spectroscopies, hydrogen nuclear magnetic resonance ((1)H NMR) spectrometry and differential scanning calorimetry (DSC) were used to characterize the prepared copolymers` structures. Polymers molecular weights were determined by gel permeation chromatography (GPC). The effect of polymer structure and composition on emission properties was studied by fluorescence (PL) spectroscopy under different irradiation wavelength. The emission energy shift due to segments with longer conjugation lengths was minor owed to the low polymerization degree achieved.

Influence of the heat treatment on the nucleation of silver nanoparticles in Tm(3+) doped PbO-GeO(2) glasses

Nucleation of silver nanoparticles (NPs) in Tm(3+) doped PbO-GeO(2) (PGO) glass is reported. The influence of the heat treatment on the nucleation of silver NPs is studied by means of transmission electron microscopy and optical spectroscopy. Two heat treatment procedures were applied in order to compare their performance. Observation of infrared-to-visible frequency upconversion (UC) luminescence of Tm(3+) ions is reported and correlated with the heat-treatment procedure. Enhancement of the UC emission for samples heat treated during various time intervals is attributed to the increased local field in the vicinity of the NPs. Quenching of the UC signal was also observed and correlated with the growth of NPs amount and size.

Montmorillonite/carbon nanocomposites prepared from sucrose for catalytic applications

Sucrose was used to prepare montmorillonite/carbon nanocomposites by calcination in a reduced atmosphere. The aim was to investigate the changes derived from varying the clay and sucrose content in the resulting material and to change the adsorption properties to evaluate its potential to be used in catalytic applications. X-ray diffraction patterns revealed the formation of an intercalated nanostructure composed of carbon-filled clay mineral layers, which was confirmed by the Fourier transform infrared spectra and thermogravimetry curves. Differences in composition and texture surface were detected by scanning electron microscopy images and were supported by viscosity measurements. These measurements were helpful in understanding why the sample prepared with the highest sucrose content presented the lowest gasoline and methylene blue adsorption results and why the highest adsorption properties were attributed to the sample with the highest clay content. Moreover, BET and BJH studies allowed understanding oleic acid catalytic conversion. Finally, a water flux simulation test was performed to determine the mechanical resistance in comparison to an activated carbon. It was found that the nanocomposites were more resistant, supporting their use in catalytic applications for a longer period of time. (C) 2011 Elsevier B.V. All rights reserved.

Thin titanium oxide films deposited by e-beam evaporation with additional rapid thermal oxidation and annealing for ISFET applications

Titanium oxide (TiO(2)) has been extensively applied in the medical area due to its proved biocompatibility with human cells [1]. This work presents the characterization of titanium oxide thin films as a potential dielectric to be applied in ion sensitive field-effect transistors. The films were obtained by rapid thermal oxidation and annealing (at 300, 600, 960 and 1200 degrees C) of thin titanium films of different thicknesses (5 nm, 10 nm and 20 nm) deposited by e-beam evaporation on silicon wafers. These films were analyzed as-deposited and after annealing in forming gas for 25 min by Ellipsometry, Fourier Transform Infrared Spectroscopy (FTIR), Raman Spectroscopy (RAMAN), Atomic Force Microscopy (AFM), Rutherford Backscattering Spectroscopy (RBS) and Ti-K edge X-ray Absorption Near Edge Structure (XANES). Thin film thickness, roughness, surface grain sizes, refractive indexes and oxygen concentration depend on the oxidation and annealing temperature. Structural characterization showed mainly presence of the crystalline rutile phase, however, other oxides such Ti(2)O(3), an interfacial SiO(2) layer between the dielectric and the substrate and the anatase crystalline phase of TiO(2) films were also identified. Electrical characteristics were obtained by means of I-V and C-V measured curves of Al/Si/TiO(x)/Al capacitors. These curves showed that the films had high dielectric constants between 12 and 33, interface charge density of about 10(10)/cm(2) and leakage current density between 1 and 10(-4) A/cm(2). Field-effect transistors were fabricated in order to analyze I(D) x V(DS) and log I(D) x Bias curves. Early voltage value of -1629 V, R(OUT) value of 215 M Omega and slope of 100 mV/dec were determined for the 20 nm TiO(x) film thermally treated at 960 degrees C. (C) 2009 Elsevier B.V. All rights reserved.

Electrochemical and spectroscopic characterization of screen-printed gold-based electrodes modified with self-assembled monolayers and Tc85 protein

This work investigates the formation of self-assembled monolayers (SAMs) of cystamine and cystamine-glutaraldehyde on a screen-printed electrode, and the immobilization of the Tc85 protein (from Trypanosoma cruzi) on these monolayers. The methods used included infrared techniques, cyclic voltammetry, and electrochemical impedance spectroscopy. The electrochemical studies were performed at pH 6.9 in 0.1 mol L(-1) phosphate buffer solution containing Fe(CN)(6)(-3/-4) redox species. The surface coverage (0) of the electrode was 0.10 (cystamine), 0.35 (cystamine-glutaraldehyde) and 0.84 (Tc85). Interpretation of electrochemical impedance spectroscopy results was based on a charge-transfer reaction involving Fe(CN)(6)(-3/-4) species at high frequencies, followed by a diffusion through the monolayers at lower frequencies. Estimates of the electrode surface coverage, active site radius, and distance between two adjacent sites assumed that charge transfer occurred at the active sites, and that there was a planar diffusion of redox species to these sites. (C) 2009 Elsevier B.V. All rights reserved.

Adsorbent new materials and composites produced in a single step

The aim of this work is the production and preliminary characterization of adsorbent new materials useful for sensor development. A new plasma chamber was simulated and designed in order to obtain multiple layers and/or composites in a single step. Plasma deposited organic fluorocompound and hexamethyldisilazane (HMDS) thin films were produced and tested as adsorbent layers. Chemical characterization used ellipsometry, Raman. infrared and X-ray photoelectron spectroscopy. Hydrophobic and oleophobic character were determined by contact angle measurements. Adsorption characteristics were evaluated using quartz crystal microbalance. Not only HMDS but also the fluorocompound can polymerize but intermixing and a double layer are only obtained in very narrow conditions. The films are adsorbent and mildly hydrophobic. Films deposited on a microchromatographic column can be used on sample pretreatment to remove and/or preconcentrate volatile organic Compounds. Therefore, with this approach it is possible to obtain films with different monomers on double layer or composites, with organic/inorganic materials or particles and use them on sample pretreatment for chemical analysis. (C) 2008 Elsevier B.V. All rights reserved.

Biogenic modified silica as a sorbent of cadmium ions: Preparation and characterization

This work describes the preparation and characterization of biogenic modified silica from rice hull ash and its use as a sorbent of cadmium ions. Thus, an agro-industrial residue has been used to produce a new adsorbent product which is able to remove toxic elements. Mesoporous biogenic silica was obtained by alkaline extraction of sodium silicate by hydrolysis with the sol-gel process, and it was modified with salen using 1,2-dichloroethane as a spacer. The surface area of the silica was measured by nitrogen adsorption/desorption analysis. Surface modification was measured by Fourier transform infrared spectroscopy. The degree of functionalization was obtained by elemental analysis. This work showed that biogenic modified silica can be produced in aqueous media from rice hull ash using a simple method, providing an alternative method for adsorbent preparation. Thermogravimetric analysis showed that the salen-modified silica is stable up to 209 C. The modified silica displays appropriate structural characteristics for an adsorbent. The cylindrical pores, open at both ends, allow free diffusion of cadmium ions to the adsorption sites on the silica surface. The surface modification increases cadmium adsorption on the silica surface 100-fold. The salen-modified silica showed specific adsorption for Cd2+ of 44.52 mg/g SiO2 at cadmium concentration of 100 mg/l.

PbO-GeO(2) rib waveguides for photonic applications

This work presents for the first time to our knowledge the fabrication and characterization of rib waveguides produced with PbO-GeO(2) (PGO) thin films. The target was manufactured using pure oxides ( 60 PbO-40 GeO(2), in wt%) and amorphous thin films were produced with the RF sputtering technique. PGO thin films present small absorption in the visible and in the near infrared and refractive index of similar to 2.0. The definition of the rib waveguide structure was made using conventional optical lithography followed by plasma etching, performed in a Reactive Ion Etching (RIE) reactor. Light propagation mode in the waveguide structure was analyzed using integrated optic simulation software. Optical loss measurements were performed to determine the propagation loss at 633 nm, for ribs with height of 70 nm and width of 3-5 mu m; experimental values around 2 dB/cm were found for the propagation loss and confirmed the theoretical calculations. The results obtained demonstrate that PGO thin films are potential candidates for application in integrated optics. Published by Elsevier B.V.

Effects of sewage sludge amendment on the properties of two Brazilian oxisols and their humic acids

The effect of sewage sludge (SS) amendment on the general properties of the top layers of a sandy and a clayey oxisols and on the nature of their humic acid (HA) fractions was evaluated by chemical and physico-chemical techniques. The amended soils, especially the sandy soil, benefited of SS amendment by increasing their pH to above neutrality and enhancing the contents of C, N, P, and Ca and cation exchange capacity. The SS-HA-like sample showed larger H and N contents and a greater aliphatic character and humification degree than the HAs isolated from non-amerided soils. The composition and structure of amended soil HAs were affected by SS application as a function of soil type and layer. In particular, N-containing groups and aliphatic structures of SS-HA-like sample appears to be partially incorporated in the amended soil HAs, and these effects were more evident in the HAs from the sandy oxisol. (C) 2007 Elsevier Ltd. All rights reserved.

Using Imaging Spectroscopy to study soil properties

Imaging Spectroscopy (IS) is a promising tool for studying soil properties in large spatial domains. Going from point to image spectrometry is not only a journey from micro to macro scales, but also a long stage where problems such as dealing with data having a low signal-to-noise level, contamination of the atmosphere, large data sets, the BRDF effect and more are often encountered. In this paper we provide an up-to-date overview of some of the case studies that have used IS technology for soil science applications. Besides a brief discussion on the advantages and disadvantages of IS for studying soils, the following cases are comprehensively discussed: soil degradation (salinity, erosion, and deposition), soil mapping and classification, soil genesis and formation, soil contamination, soil water content, and soil swelling. We review these case studies and suggest that the 15 data be provided to the end-users as real reflectance and not as raw data and with better signal-to-noise ratios than presently exist. This is because converting the raw data into reflectance is a complicated stage that requires experience, knowledge, and specific infrastructures not available to many users, whereas quantitative spectral models require good quality data. These limitations serve as a barrier that impedes potential end-users, inhibiting researchers from trying this technique for their needs. The paper ends with a general call to the soil science audience to extend the utilization of the IS technique, and it provides some ideas on how to propel this technology forward to enable its widespread adoption in order to achieve a breakthrough in the field of soil science and remote sensing. (C) 2009 Elsevier Inc. All rights reserved.

Leaf area index estimation with MODIS reflectance time series and model inversion during full rotations of Eucalyptus plantations

The leaf area index (LAI) of fast-growing Eucalyptus plantations is highly dynamic both seasonally and interannually, and is spatially variable depending on pedo-climatic conditions. LAI is very important in determining the carbon and water balance of a stand, but is difficult to measure during a complete stand rotation and at large scales. Remote-sensing methods allowing the retrieval of LAI time series with accuracy and precision are therefore necessary. Here, we tested two methods for LAI estimation from MODIS 250m resolution red and near-infrared (NIR) reflectance time series. The first method involved the inversion of a coupled model of leaf reflectance and transmittance (PROSPECT4), soil reflectance (SOILSPECT) and canopy radiative transfer (4SAIL2). Model parameters other than the LAI were either fixed to measured constant values, or allowed to vary seasonally and/or with stand age according to trends observed in field measurements. The LAI was assumed to vary throughout the rotation following a series of alternately increasing and decreasing sigmoid curves. The parameters of each sigmoid curve that allowed the best fit of simulated canopy reflectance to MODIS red and NIR reflectance data were obtained by minimization techniques. The second method was based on a linear relationship between the LAI and values of the GEneralized Soil Adjusted Vegetation Index (GESAVI), which was calibrated using destructive LAI measurements made at two seasons, on Eucalyptus stands of different ages and productivity levels. The ability of each approach to reproduce field-measured LAI values was assessed, and uncertainty on results and parameter sensitivities were examined. Both methods offered a good fit between measured and estimated LAI (R(2) = 0.80 and R(2) = 0.62 for model inversion and GESAVI-based methods, respectively), but the GESAVI-based method overestimated the LAI at young ages. (C) 2010 Elsevier Inc. All rights reserved.

Simultaneous determination of econazole nitrate, main impurities and preservatives in cream formulation by high performance liquid chromatography

A reversed-phase high performance liquid chromatographic (RP-HPLC) method for determination of econazole nitrate, preservatives (methylparaben and propylparaben) and its main impurities (4-chlorobenzl alcohol and alpha-(2,4-dicholorophenyl)-1H-imidazole-1-ethanol) in cream formulations, has been developed and validated. Separation was achieved on a column Bondclone (R) C18 (300 mm x 3.9 mm i.d., 10 mu m) using a gradient method with mobile phase composed of methanol and water. The flow rate was 1.4 mL min(-1), temperature of the column was 25 C and the detection was made at 220 nm. Miconazole nitrate was used as an internal standard. The total run time was less than 15 min, The analytical curves presented coefficient of correlation upper to 0.99 and detection and quantitation limits were calculated for all molecules. Excellent accuracy and precision were obtained for econazole nitrate. Recoveries varied from 97.9 to 102.3% and intra- and inter-day precisions, calculated as relative standard deviation (R.S.D), were lower than 2.2%. Specificity, robustness and assay for econazole nitrate were also determined. The method allowed the quantitative determination of econazole nitrate, its impurities and preservatives and could be applied as a stability-indicating method for econazole nitrate in cream formulations. (C) 2008 Elsevier B.V. All rights reserved.

Obtention and Evaluation of Inclusion Complexes of Furosemide with beta-ciclodextrin and hidroxipropil-beta-ciclodextrin: Effects on Drug`s Dissolution Properties

Obtention and Evaluation of Inclusion Complexes of Furosemide with beta-ciclodextrin and hidroxipropil-beta-ciclodextrin: Effects on Drug`s Dissolution Properties. The purpose of this study was to prepare, characterize and evaluate the dissolution behavior of inclusion complexes of furosemide with beta-cyclodextrin (beta-CD) and hydroxypropyl-beta-cyclodextrin (HP-beta-CD). Solid complexes of furosemide with P-CD and-HP-beta-CD were prepared by using a freeze-drying method. Physical mixtures were prepared for comparison. The inclusion complexes were characterized by differential scanning calorimetry (DSC), Infrared (IR) and dissolution test. ""In vitro"" dissolutions assays were performed at pH 1,2; pH 4,5 and pH 6,8 media for a 60 min period. Statistical analysis employing ANOVA and Tukey`s Test, for the dissolution efficiency values (ED%), showed that complexation of furosemide with both cyclodextrins improved significantly ED% of the drug in all tested media, suggesting a minor pH influence on dissolution properties of the drug.

Development and validation of a method for quantitative determination of econazole nitrate in cream formulation by capillary zone electrophoresis

A simple, fast, inexpensive and reliable capillary zone electrophoresis (CZE) method for the determination of econazole nitrate in cream formulations has been developed and validated. Optimum conditions comprised a pH 2.5 phosphate buffer at 20 mmol L(-1) concentration, +30 kV applied voltage in a 31.5 cm x 50 mu m I.D. capillary. Direct UV detection at 200 nm led to an adequate sensitivity without interference from sample excipients. A single extraction step of the cream sample in hydrochloric acid was performed prior to injection. Imidazole (100 mu g mL(-1)) was used as internal standard. Econazole nitrate migrates in approximately 1.2 min. The analytical curve presented a coefficient of correlation of 0.9995. Detection and quantitation limits were 1.85 and 5.62 mu g mL(-1), respectively. Excellent accuracy and precision were obtained. Recoveries varied from 98.1 to 102.5% and intra- and inter-day precisions, calculated as relative standard deviation (RSD), were better than 2.0%. The proposed CZE method presented advantageous performance characteristics and it can be considered suitable for the quality control of econazole nitrate cream formulations. (c) 2008 Elsevier B.V. All rights reserved.