Using Polycarbonate Membranes as Templates for the Preparation of Au Nanostructures for Surface-Enhanced Raman Scattering

Polycarbonate membranes (PCM) of various pores sizes (400, 200, 100 and 50 nm) were used as templates for gold deposition. The electrodeposition from gold ions resulted in the formation of gold nanotubes when large pores size PCMs (400 and 200 nm) were used. On the other hand, gold nanowires were predominant for the PCMs with smaller pores size (100 and 50 nm). Surface-enhanced Raman scattering (SERS) from the probe molecule 4-mercaptopyridine (4-MPy) was obtained from all these nanostructures. The SERS efficiency of the substrates produced using the PC M templates were compared to two commonly used SERS platforms: a roughened gold electrode and gold nanostructures electrodeposited through organized polystyrene spheres (PSS). The SERS signal of the probe molecule increased as the pore diameter of the PCM template decreased. Moreover, the SERS efficiency from the nanostructures produced using 50 nm PCM templates was four and two times better than the signal from the roughened gold electrode and the PSS template, respectively. The SERS substrates prepared using PCM templates were more homogenous over a larger area (ca. 1 cm(2)), presented better spatial and sample to sample reproducibility than the other substrates. These results show that SERS substrates prepared using PCM templates are promising for the fabrication of planar SERS platforms for analytical/bioanalytical applications.

Structural and surface properties of thermally prepared Ti/RhxTi(1-x)Oy electrodes: I - influence of preparation parameters

Electrodes of RhxTi(1-x) O-y nominal composition were prepared by thermal decomposition of the chloride or nitrate precursor salts dissolved in strongly acidic medium and applied by brush to both sides of a Tidegrees support. A systematic study of the influence of calcination temperature and time as well as oxygen flux was conducted. The coatings were characterised by SEM, EDAX, XRD, open circuit potential measurements and cyclic voltammetry (CV). Visible-ultraviolet spectrophotometry was employed to identify the chemical form of the precursor in solution while thermogravimetric analysis (TGA) was used to assess the decomposition temperature ranges. Optimisation of the coating preparation parameters showed coatings obtained from [Rh(H2O)(6)](NO3)(3) precursor dissolved in HNO3 1:2 (v/v) and fired at 430 degreesC for 2 h in a 5 1 min (-1) oxygen stream-furnished stable electrodes having the highest electrochemically active surface area. (C) 2002 Elsevier B.V. Ltd. All rights reserved.

Preparation of ceramic membranes from surface modified tin oxide nanoparticles

The preparation of crack-free SnO2 supported membranes requires the development of new strategies of synthesis capable to allow controlled changes of surface chemistry and to improve the processability of supported layers. In this way, the controlled modification of the SnO2 nanoparticle surface by adding capping molecules like Tiron(R) ((OH)(2)C6H2(SO3Na)(2)) during the sol-gel process was studied, aiming to obtain high performance membranes. Colloidal suspensions were prepared by hydrolyzing SnCl4.5H(2)O aqueous solution with NH4OH in presence of Tiron(R). The effect of the amount of Tiro(R) (from I to 20 wt.%) on the structural features of nanoparticles, powder redispersability and particle-solution interface properties was investigated by X-ray powder diffraction (XRPD), extended X-ray absorption fine structure (EXAFS), quasi-elastic light scattering and electrophoretic mobility measurements. XRPD and EXAFS results showed that the addition of Tiron(R) up to 20 wt.% to colloidal suspensions does not affect the crystallite size of SnO2 primary particles, determined around 2-3 nm. This value is comparable to the hydrodynamic size measured after redispersion of powder prepared with amount of Tiro(R) higher than 7.5 wt.%, indicating the absence of condensation reactions between primary particles after the initial precipitation step. As a consequence the powder with amount of Tiron(R) > 7.5 wt.%, can be fully redispersed in aqueous solution at pH greater than or equal to I I until a nanoparticle concentration of 6 vol.%. The electrophoresis measurements showed a decrease of the isoelectric point by increasing the amount of grafted Tiron(R) at the SnO2 nanoparticle surface, resulting in negatively charged particle-solution interface in all the studied pH range (2-11). These features govern the gelation process favoring the preparation of crack-free SnO2 supported membranes. The control exercised by Tiron(R) modifying agent in the aggregation process allows the fine-tuning of the porosity, from 0.124 to 0.065 cm(3) g(-1), and mean pore size, from 6.4 to 1.9 nm, as the amount of grafted molecules increases from 0 to 10 wt.%. In consequence, the membrane cut-off determined by filtration of polyethylene glycol standard solutions can be screened from 1500 to 3500 g mol(-1). (C) 2002 Elsevier B.V. B.V. All rights reserved.

PREPARATION AND CHARACTERIZATION OF TI(IV) OXIDE GRAFTED ONTO SILICA ON A SILICA-GEL SURFACE

Silica gel with a surface area of 500 m2g-1 and an average pore diameter of 60 angstrom was chemically modified with Ti(IV) oxide using the grafting method. The amount of metal oxide attached to the surface was 1.8.10(-3) mol g-1. The X-ray photoelectron spectra showed that the metal ion species on the surface are Ti(IV) in TiO2 and MTiO3 (M = Ca2+, Sr2+, Ba2+ and Pb2+), i.e. they have the binding energy of Ti2p3/2 = 458.7 eV. The dehydration of the solid at higher temperature increased the O(II)/Ti (O(II) = oxygen bound to titanium atom) ratio, presumably due to a reticulation of the hydrous Ti(IV) oxide on the silica surface at higher temperatures. Migration of Ti(IV) into the silica gel matrix was observed but the specific surface area was not significantly changed.

Corn productivity in function of surface application of lime in differents management systems and cultural preparation

The evaluation of technologies employed at the agricultural production system such as crop rotation and soil preparation, both associated with crop-livestock integration, is crucial. Therefore, the aim of the present study was to evaluate the incorporation of lime for three no-tillage systems and cultural managements in system of crop-livestock integration, with emphasis on corn grain yield. The experiment was conducted from January 2003 to April 2005 at Selvíria city, MS, in Dystroferric Red Latosol, clay texture. The experimental design was randomized blocks with split plots consisted of three main treatments, aimed the soil physics conditioning and the incorporation of lime: PD - No-no-tillage; CM - minimum no-tillage, and PC - conventional no-tillage; and of two secondary treatments related to the management: rotation and crop succession, with four replications. Data on agronomic traits of maize were analyzed: plant height, stem diameter, height of the first spike insertion, 100 grains weight and grain yield. The results showed that the maize produced under the system of crop-livestock integration is quite feasible, showing that grain yields are comparable to averages in the region and the different soil physical conditioning and incorporation of lime did not influence the corn yield as well as the cultural managements, rotation and succession, did not affect the maize crop behavior after two years of cultivation.

New hybrid materials based on the grafting of Pd(II)-amino complexes on the graphitic surface of AC: preparation, structures and catalytic properties

A novel procedure for the preparation of solid Pd(II)-based catalysts consisting of the anchorage of designed Pd(II)-complexes on an activated carbon (AC) surface is reported. Two molecules of the Ar–S–F type (where Ar is a plane-pyrimidine moiety, F a Pd(II)-ligand and S an aliphatic linker) differing in F, were grafted on AC by π–π stacking of the Ar moiety and the graphene planes of the AC, thus favouring the retaining of the metal-complexing ability of F. Adsorption of Pd(II) by the AC/Ar–S–F hybrids occurs via Pd(II)-complexation by F. After deep characterization, the catalytic activities of the AC/Ar–S–F/Pd(II) hybrids on the hydrogenation of 1-octene in methanol as a catalytic test were evaluated. 100% conversion to n-octane at T = 323.1 K and P = 15 bar, was obtained with both catalysts and most of Pd(II) was reduced to Pd(0) nanoparticles, which remained on the AC surface. Reusing the catalysts in three additional cycles reveals that the catalyst bearing the F ligand with a larger Pd-complexing ability showed no loss of activity (100% conversion to n-octane) which is assigned to its larger structural stability. The catalyst with the weaker F ligand underwent a progressive loss of activity (from 100% to 79% in four cycles), due to the constant aggregation of the Pd(0) nanoparticles. Milder conditions, T = 303.1 K and P = 1.5 bar, prevent the aggregation of the Pd(0) nanoparticles in this catalyst allowing the retention of the high catalytic efficiency (100% conversion) in four reaction cycles.

Preparation of environmental monitoring plan pattern for surface water quality in Iran (Case study: Gharehsou River)

Using water quality management programs is a necessary and inevitable way for preservation and sustainable use of water resources. One of the important issues in determining the quality of water in rivers is designing effective quality control networks, so that the measured quality variables in these stations are, as far as possible, indicative of overall changes in water quality. One of the methods to achieve this goal is increasing the number of quality monitoring stations and sampling instances. Since this will dramatically increase the annual cost of monitoring, deciding on which stations and parameters are the most important ones, along with increasing the instances of sampling, in a way that shows maximum change in the system under study can affect the future decision-making processes for optimizing the efficacy of extant monitoring network, removing or adding new stations or parameters and decreasing or increasing sampling instances. This end, the efficiency of multivariate statistical procedures was studied in this thesis. Multivariate statistical procedure, with regard to its features, can be used as a practical and useful method in recognizing and analyzing rivers’ pollution and consequently in understanding, reasoning, controlling, and correct decision-making in water quality management. This research was carried out using multivariate statistical techniques for analyzing the quality of water and monitoring the variables affecting its quality in Gharasou river, in Ardabil province in northwest of Iran. During a year, 28 physical and chemical parameters were sampled in 11 stations. The results of these measurements were analyzed by multivariate procedures such as: Cluster Analysis (CA), Principal Component Analysis (PCA), Factor Analysis (FA), and Discriminant Analysis (DA). Based on the findings from cluster analysis, principal component analysis, and factor analysis the stations were divided into three groups of highly polluted (HP), moderately polluted (MP), and less polluted (LP) stations Thus, this study illustrates the usefulness of multivariate statistical techniques for analysis and interpretation of complex data sets, and in water quality assessment, identification of pollution sources/factors and understanding spatial variations in water quality for effective river water quality management. This study also shows the effectiveness of these techniques for getting better information about the water quality and design of monitoring network for effective management of water resources. Therefore, based on the results, Gharasou river water quality monitoring program was developed and presented.

Well-controlled preparation of evenly distributed nanoporous HOPG surface via diazonium salt assisted electrochemical etching process

Evenly distributed nanoporous highly oriented pyrolytic graphite (HOPG) surfaces with controllable pore size were successfully prepared via diazonium salt assisted electrochemical etching method. The porous HOPG was investigated by atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) Raman spectroscopy and X-ray diffraction. The size of these pores can be tuned by manipulating the electrochemical etching time. These porous HOPG substrates also demonstrated the enhanced electrocatalytical behaviour and were employed as benign arena for the immobilization of Ru(bpy)32+ for electrochemiluminescence (ECL) sensing applications.