Determination of copper, iron, nickel and zinc in gasoline by FAAS after sorption and preconcentration on silica modified with 2-aminotiazole groups

Silica gel chemically modified with 2-aminotiazole groups (SiAT), was used for preconcentration of cupper, zinc, nickel and iron from gasoline, normally used as a engine fuel. Surface characteristics and surface area of the silica gel were obtained before and after chemical modification using FT-IR, Kjeldhal and surface area analysis (B.E.T.). The retention and recovery of the analyte elements were studied by applying batch and column techniques. The experimental parameters, such as shaking time in batch technique, flow rate and concentration of the eluent (HCl-0.25-2.00 mol 1(-1)) and the amount of silica, on retention and elution, have been investigated. Detection limits of the method for cupper, iron, nickel and zinc are 0.8, 3, 2 and 0.1 mug 1(-1), respectively. The sorption-desorption of the studied metal ions made possible the development of a preconcentration method for metal ions at trace level in gasoline using flame AAS for their quantification. (C) 2004 Published by Elsevier Ltd.

Determination of Cd(II), Cu(II) and Ni(II) in aqueous samples by ICP-OES after on-line preconcentration in column packed with silica modified with 2-aminothiazole

This work describes the synthesis and characterization of 2-aminothiazole modified silica gel (SiAT) and the studies of adsorption and pre-concentration (in batch and using a flow-injection system coupled with optical emission spectrometer) of Cd(II), Cu(II) and Ni(II) in aqueous medium. The adsorption capacity for each metal ions in mmolg(-1) was: Cu(II) = 1.18, Ni(II) = 1.15 and Cd(II) = 1.10. The results obtained in the flow experiments showed about 100% of recovering of the metal ions adsorbed in a mini-column packed with 100 mg of SiAT, using 100 mu L of 2.0 mol L-1 HCl solution as eluent. The quantitative sorption-desorption of the metal ions made possible the application of a flow-injection system in the pre-concentration and quantification by ICP-OES of metal ions at trace level in natural water samples.

A solid paraffin-based carbon paste electrode modified with 2-aminothiazole organofunctionalized silica for differential pulse adsorptive stripping analysis of nickel in ethanol fuel

A solid paraffin-based carbon paste electrode modified with 2-aminothiazole organofunctionalized silica (SiAt-SPCPE) was applied to Ni2+ determination in commercial ethanol fuel samples. The proposed method comprised four steps: (1) Ni2+ preconcentration at open circuit potential directly in the ethanol fuel sample, (2) transference of the electrode to an electrochemical cell containing DMG, (3) differential pulse voltammogram registering and (4) surface regeneration by polishing the electrode. The proposed method combines the high Ni2+ adsorption capacity presented by 2-aminothiazole organofunctionalized silica with the electrochemical properties of the Ni(DMG)2 complex, whose electrochemical reduction provides the analytical signal.All experimental parameters involved in the proposed method were optimized. Using a preconcentration time of 20 min, it was obtained a linear range from 7.5 x 10(-9) to 1.0 x 10(-6) mol L-1 with detection limit of 2.0 x 10(-9) mol L-1. Recovery values between 96.5 and 102.4% were obtained for commercial samples spiked with 1.0 mu mol L-1 Ni2+ and the developed electrode was totally stable in ethanolic solutions. The contents of Ni2+ found in the commercial samples using the proposed method were compared to those obtained by graphite furnace atomic absorption spectroscopy by using the F- and t-test. Neither the F- nor t-values exceeded the critical values at 95% confidence level, confirming that there are not statistical differences between the results obtained by both methods. These results indicate that the developed electrode can be successfully employed to reliable Ni2+ determination in commercial ethanol fuel samples without any sample pretreatment or dilution step. (c) 2006 Elsevier B.V. All rights reserved.

(1-x)PMN-xPT ceramics prepared by conventional and modified columbite route: Effect on electrical properties

This study aims to demonstrate how the chemical homogeneity of B cations affects the microstructure and electrical responses of (1-x) PMN-xPT ceramics. Two methodologies were employed to synthesize three different compositions, with x assuming the values 0.10, 0.28, and 0.35. If compared to conventional method, the Ti-modified columbite route, which is characterized by higher B cation homogeneity, leads to PMN-PT powders and ceramics with lower content of PNT pyrochlore phase and, for 0.65PMN-0.35PT composition, minor amount of tetragonal phase is found. Conclusively, PMN-PT ceramics obtained by modified route favors B cations homogeneity, enhancing the dielectric, ferroelectric and piezoelectric properties.

Effect of lithium additive on the microstructure and electrical responses of 0.9PMN-0.1PT ceramics

Structural effects of lithium additive on 0.9PMN-0.1PT powders prepared by Ti-modified columbite route were studied. The substitution of Li+ ions for Mg2+ ions in the B-site sub-lattice of 0.9PMN-0.1PT perovskite structure was explained in terms of lead and oxygen vacancies generation originated as consequence of the ionic compensation of negatively charged Li'(Mg) sites. The rise in mass transport as consequence of the increasing of Pb2+ and O2- vacancies produces more agglomerated particles during the powder synthesis and changes the mechanical characteristics between grain and grain boundary of sintered ceramic. The relation between K-m and T-m values, the difference between ionic radii of B cation and the molar volume were used to explain the changes in the relaxor behavior and diffusiveness of phase transition as function of lithium doping, which are corroborated by the results obtained through the ferroelectric characterization.

Determination of metal ions in natural waters by flame-AAS after preconcentration on a 5-amino-1,3,4-thiadiazole-2-thiol modified silica gel.

5-amino-1,3,4-thiadiazole-2-thiol groups attached on a silica gel surface have been used for adsorption of Cd(II), Co(II), Cu(II), Fe(III), Ni(II), Pb(II) and Zn(II) from aqueous solutions. The adsorption capacities for each metal ion were (in mmol.g(-1)): Cd(II)= 0.35, Co(II)= 0.10, Cu(II)= 0.15, Fe(III)= 0.20, Hg(Il)= 0.46, Ni(II)= 0.16, Pb(II)= 0.13 and Zn(II)= 0.15. The modified silica gel was applied in the preconcentration and quantification of trace level metal ions present in water samples (river, and bog water).

Copper determination in ethanol fuel by differential pulse anodic stripping voltammetry at a solid paraffin-based carbon paste electrode modified with 2-aminothiazole organofunctionalized silica

Solid paraffin-based carbon paste electrodes modified with 2-aminothiazole organofunctionalized silica have been applied to the anodic stripping determination of copper ions in ethanol fuel samples without any sample treatment. The proposed method comprised four steps: (1) copper ions preconcentration at open circuit potential directly in the ethanol fuel sample; (2) exchange of the solution and immediate cathodic reduction of the absorbate at controlled potential; (3) differential pulse anodic stripping voltammetry; (4) electrochemical surface regeneration by applying a positive potential in acid media. Factors affecting the preconcentration, reduction and stripping steps were investigated and the optimum conditions were employed to develop the analytical procedure. Using a preconcentration time of 20 min and reduction time of 120 s at -0.3 V versus Ag/AgCl(sat) a linear range from 7.5 x 10(-8) to 2.5 x 10(-6) mol L(-1) with detection limit of 3.1 x 10(-8) mol L(-1) was obtained. Interference studies have shown a decrease in the interference effect according to the sequence: Ni > Zn > Cd > Pb > Fe. However, the interference effects of these ions have not forbidden the application of the proposed method. Recovery values between 98.8 and 102.3% were obtained for synthetic samples spiked with known amounts of Cu(2+) and interfering metallic ions. The developed electrode was successfully applied to the determination of Cu(2+) in commercial ethanol fuel samples. The results were compared to those obtained by flame atomic absorption spectroscopy by using the F-test and t-test. Neither F-value nor t-value have exceeded the critical values at 95% confidence level, confirming that there are no significant differences between the results obtained by both methods. (c) 2006 Elsevier B.V. All rights reserved.

Characterization of silica-carbon mesoporous matrix with embedded nickel nanoparticles synthesized by the polymeric precursor method

Nickel nanoparticles into silica-carbon matrix composites were prepared by using the polymeric precursor method. The effects of the polyester type and the time of pyrolysis on the mesoporosity and nickel particle dispersion into non-aqueous amorphous silica-carbon matrix were investigated by thermogravimetric analysis, adsorption/desorption isotherms and TEM. A well-dispersed metallic phase could be only obtained by using ethylene glycol. Weightier polyesters affected the pyrolysis process due to a combination of more amounts of carbonaceous residues and delaying of pyrolysis process. The post-pyrolyzed composites were successfully cleaned at 200 degrees C for I h in oxygen atmosphere leading to an increase in the surface area and without the occurrence of carbon combustion or nickel nanoparticles oxidation. The matrix composites presented predominantly mesoporous with pore size well defined in 38 angstrom, mainly when tetraethylene glycol was used as polymerizing agent. (C) 2007 Elsevier B.V. All rights reserved.

Determination of Cu, Ni, and Zn in fuel ethanol by FAAS after enrichment in column packed with 2-aminothiazole-modified silica gel

This work describes the synthesis and characterization of 2-aminothiazole-modified silica gel (SiAT), as well as its application for preconcentration (in batch and column technique) of Cu(II), Ni(II) and Zn(II) in ethanol medium. The adsorption capacities of SiAT determined for each metal ion were (mmol g(-1)): Cu(II)=1.20, Ni(II)=1.10 and Zn(II)=0.90. In addition, results obtained in flow experiments, showed a recovery of ca. 100% of the metal ions adsorbed in a column packed with 500 mg of SiAT. The eluent was 2.0 mol L-1 HCl. The sorption-desorption of the studied metal ions made possible the development of a preconcentration method for metal ions at trace level in fuel ethanol using flame AAS for their quantification.

Surface Roughness and Bacterial Adherence to Resin Composites and Ceramics

Purpose: The aim of this study was to evaluate the surface roughness and the in vitro adherence of Streptococcus mutans to indirect aesthetic restorative materials that are uncoated with saliva.Materials and Methods: Four groups of restorative materials were evaluated according to material type: (1) microparticulate feldspathic ceramic; (2) leucite-reinforced feldspathic ceramic; (3) microhybrid resin composite and (4) microfilled resin composite. Twenty standardised samples of each material were produced. Roughness analysis (Ra, n = 10) was performed using a roughness analyser. Adhesion tests (n = 10) were carried out in 24-well plates; colony-forming units (CFU/mL) were evaluated. The mean values of roughness (mu m) and adherence (CFU/mL) for each group were subjected to an analysis of variance and a Tukey test.Results: The leucite-reinforced feldspathic ceramic was rougher and presented higher bacterial adherence than the microparticulate feldspathic ceramic. The resin composites were similar with regard to surface roughness and bacterial adherence.Conclusions: The microhybrid and microfilled resin composites were similar and the leucite-reinforced feldspathic ceramic was rougher and presented higher bacterial adherence than the microparticulate feldspathic ceramic.

Effect of the addition of silanated silica on the mechanical properties of microwave heat-cured acrylic resin

Effect of the addition of silanated silica on the mechanical properties of microwave heat-cured acrylic resinObjectives: The purpose of this study was to evaluate the flexural strength and Vickers hardness of a microwave energy heat-cured acrylic resin by adding different concentrations of silane surface-treated nanoparticle silica.Methods: Acrylic resin specimens with dimensions of 65 x 10 x 2.5 mm were formed and divided into five experimental groups (n = 10) according to the silica concentration added to the acrylic resin mass (weight %) prior to polymerisation : G1, without silica; G2, 0.1% silica; G3, 0.5% silica; G4, 1.0% silica; and G5, 5.0% silica. The specimens were submitted to a three-point flexural strength test and to the Vickers hardness test (HVN). The data obtained were statistically analysed by ANOVA and the Tukey test (alpha = 0.05).Results: Regarding flexural strength, G5 differed from the other experimental groups (G1, G2, G3 and G4) presenting the lowest mean, while G4 presented a significantly higher mean, with the exception of group G3. Regarding Vickers hardness, a decrease in values was observed, in which G1 presented the highest hardness compared with the other experimental groups.Conclusion: Incorporating surface-treated silica resulted in direct benefits in the flexural strength of the acrylic resin activated by microwave energy; however, similar results were not achieved for hardness.

Flexural Strength of Four Adhesive Fixed Dental Prostheses of Composite Resin Reinforced with Glass Fiber

Purpose: To evaluate the flexural strength of two fixed dental prosthesis (FDP) designs simulating frameworks of adhesive fixed partial prostheses, reinforced or not by glass fiber.Materials and Methods: Forty specimens, made with composite resin, were divided into 4 groups according to the framework design and the presence of fiber reinforcement: A1 - occlusal support; A2: occlusal support + glass fiber; B1: occlusal and proximal supports; B2: occlusal and proximal supports + glass fiber. The specimens were subjected to the three-point bending test, and the data were submitted to two-way ANOVA and Tukey's test (5%).Results: Group A2 (97.9 +/- 38 N) was statistically significantly different from all other experimental groups, presenting a significantly lower mean flexural strength.Conclusion: The use of glass fibers did not improve the flexural strength of composite resin, and designs with occlusal and proximal supports presented better results than designs simulating only occlusal support.

Effect of Static and Cyclic Loading on Ceramic Laminate Veneers Adhered to Teeth with and Without Aged Composite Restorations

Purpose: Existing composite restorations on teeth are often remade prior to the cementation of fixed dental prostheses. The aim of this study was to evaluate the effect of static and cyclic loading on ceramic laminate veneers adhered to aged resin composite restorations.Materials and Methods: Eighty sound maxillary incisors were collected and randomly divided into four groups: group 1: control group, no restorations; group 2: two Class III restorations; group 3: two Class IV restorations; group 4: complete composite substrate. Standard composite restorations were made using a microhybrid resin composite (Anterior Shine). Restored teeth were subjected to thermocycling (6000 cycles). Window preparations were made on the labial surface of the teeth for ceramic laminate fabrication (Empress II). Teeth were conditioned using an etch-and-rinse system. Existing composite restorations representing the aged composites were silica coated (CoJet) and silanized (ESPE-Sil). Ceramic laminates were cemented using a bis-GMA-based cement (Variolink Veneer). The specimens were randomly divided into two groups and were subjected to either static (groups 1a, 2a, 3a, 4a) or cyclic loading (groups 1b, 2b, 3b, 4b). Failure type and location after loading were classified. Data were analyzed using one-way ANOVA and Tukey's test.Results: Significantly higher fracture strength was obtained in group 4 (330 +/- 81 N) compared to the controls in group 1 (179 +/- 120 N) (one-way ANOVA, p < 0.05). Group lb survived a lower mean number of cyclic loads (672,820 cycles) than teeth of groups 2b to 4b (846x10(3) to 873x10(3) cycles). Failure type evaluation after the fracture test showed predominantly adhesive failures between dentin and cement, but after cyclic loading, more cohesive fractures in the ceramic were seen.Conclusion: Ceramic laminate veneers bonded to conditioned aged composite restorations provided favorable results. Surface conditioning of existing restorations may eliminate the necessity of removing aged composite restorations.