Comparative study between EDXRF and ASTM E572 methods using two-way ANOVA

Comparison with reference method is one of the necessary requirements for the validation of non-standard methods. This comparison was made using the experiment planning technique with two-way ANOVA. In ANOVA, the results obtained using the EDXRF method, to be validated, were compared with the results obtained using the ASTM E572-13 standard test method. Fisher's tests (F -test) were used to comparative study between of the elements: molybdenum, niobium, copper, nickel, manganese, chromium and vanadium. All F -tests of the elements indicate that the null hypothesis (Ho) has not been rejected. As a result, there is no significant difference between the methods compared. Therefore, according to this study, it is concluded that the EDXRF method was approved in this method comparison requirement

Dynamic behaviour of an electrolyser with a two phase solid-liquid electrolyte : Part I : spectral analysis of potential fluctuations

The dynamic behaviour of a simplified electrolyser with a two phase solid-liquid electrolyte was investigated. The current-voltage curve and the impedance of the working electrode (current collector) was measured. In addition the fluctuations of the working electrode potential and of the electrolyte resistance close to the electrode were analysed, especially by spectral analysis. Conductive zinc-coated polystyrene beads and insulating glass beads were compared. For glass beads the kinetics were controlled by ohmic drop fluctuations due to the collisions of the beads onto the collector. With zinc beads the charge exchanges between the beads and the current collector were also observed and contributed to the potential fluctuations. A complementary analysis of the elementary potential and electrolyte resistance transients will be reported in Part II; the electrochemical behaviour of the collector will then be modelled

Effect of operational parameters and Pd/In catalyst in the reduction of nitrate using copper electrode

Water with high concentration of nitrate may cause damage to health and to the environment. This study investigated how concentration, current density, flow, pH, the use of Pd/In catalyst and operating mode (constant current density and constant cell potential) have an influence in the electrochemical reduction of nitrate and in the formation of gaseous compounds using copper electrode. Experiments were performed in two-compartment electrolytic cells separated by a cationic membrane with nitrate model solutions prepared as a surrogate of concentrated brines from membrane desalination plants. The results show that the electroreduction process has potential for reduction of nitrate and that it is influenced by the operational conditions. The best conditions found for the treatment - with satisfactory reduction of nitrate, formation of compounds and reproducibility - were at nitrate concentrations of 600 and 1000 mg.L-1, current density of 1.1 mA.cm-2 and without pH control, since in these conditions the production of gaseous compounds is higher than the production of nitrite. When Pd/In catalyst was used, the nitrate reduction was 50% after 6 hours of experiment and the predominant product were gaseous compounds. When compared to the experiment without the catalyst, the arrangement with Pd/In was the most efficient one.Fil: Beltrame, Thiago Favarini. Ufrgds Lacor; BrasilFil: Coelho, Vanessa. Ufrgds Lacor; BrasilFil: Marder, Luciano. Ufrgds Lacor; BrasilFil: Ferreira, Jane Zoppas. Ufrgds Lacor; BrasilFil: Marchesini, Fernanda Albana. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Santa Fe. Instituto de Investigaciones en Catálisis y Petroquímica ; ArgentinaFil: Bernardes, Andrea Moura. Ufrgds Lacor; Brasi

Obtainment and characterization of a silicon alkoxides-based coating applied to a substrate of stainless steel 316L for use in biomaterials

The silicon alkoxides-based coating is an alternative to control the release of cytotoxic ions through metal implants. This study evaluated the influence of the number of layers of a hybrid coating on the surface of austenitic stainless steel AISI 316L on the corrosion resistance. This coating was produced from the precursors of silicon alkoxides 3-(trimethoxysilyl)propyl methacrylate (MAP) and tetraethoxisylane (TEOS) obtained by sol-gel process, and easily applied by dip-coating. Results indicated that a single layer of coating in the substrate showed a better protection than two layers. This single layer developed by the combination of the precursors TEOS-MAP was enough to create a compact and uniform film with good adherence to AISI 316L and higher electrochemical development. A single layer of TEOS-MAP coating is more adequate as a protective coating for the AISI 361L than the sample subjected to two layers and the non-coated substrate, because this film ensures its integrity in an aggressive environment

Computational image analysis as an alternative tool for the evaluation of corrosion in salt spray test

The current standards for evaluating corrosion during salt spray tests rely on the visual analysis of the specimens, and this may be a limitation when higher resolution quantitative outputs are desired. In this work, computational image analysis was used to measure the area affected by corrosion during salt spray tests with aluminum alloy, copper, carbon steel and galvanized steel plates. The software ImageJ was used to select and measure the corroded areas differentiating the corrosion products from the metals uncorroded surfaces according to their different colors. With ten measurements for each selected exposure time, a 95 % confidence interval was calculated for each material and time of exposure, giving an indication of the precision of the estimated corroded area. These data were compared with a visual inspection carried out by an experienced technician. The results indicate that computational image analysis may be a powerful tool to obtain higher resolution in the results interpretation in comparison with the standard visual analysis

Influence of concentration and pH of hexafluorozirconic acid on corrosion resistance of anodized AA7075-T6

7XXX aluminum alloys show high mechanical resistance and low weight, both required properties for aircraft industry. Anodizing is an electrolytical process typically used to improve the corrosion resistance of aluminum alloys, through which a thicker and porous oxide is formed. Boiling water is used as a common sealing method to the anodic layer; however, it implies energy expenditure. In this work, a two-step coating system was performed: anodizing in tartaric-sulphuric acid and a post-treatment with a Zr-based conversion coating, obtained at room temperature by immersion in hexafluorozirconic acid (H2 ZrF6 ). To establish the best condition for coating formation on the aluminum oxide layer, different concentration and pH values of the H2 ZrF6 solution were studied. Morphological and chemical analyses were performed respectively by SEM and EDS. The corrosion resistance evaluation was carried out by EIS in 0.5 M NaCl. Heterogeneity was observed in the obtained coatings. However, the samples treated with H2 ZrF6 had a higher corrosion resistance than unsealed samples. The best concentration and pH range observed for the H2 ZrF6 solution were 1 % and 3 to 3.5, respectively. Under these conditions, a greater corrosion resistance was evidenced in comparison to that obtained with boiling water sealing

NiP/SiC composite coatings: the effects of particles on the electrochemical behaviour

NiP/SiC (17 at.% P) composite coatings were prepared by electrodeposition from a Brenner type plating bath containing SiC particles. Cyclic voltammetry and immersion time were used to evaluate the electrochemical behaviour of these coatings. The results showed that the presence of SiC particles in NiP alloy increased corrosion properties, because the exposed area of the metallic matrix was reduced due to its recovering by SiC particles. However, the current densities developed by the NiP/SiC composite coatings increased with increasing amount of incorporated particles, and such effect is more remarkable for small particles, after heat treatment and when the systems are polarized

Electrochemical behavior during the zirconium conversion coating formation on AISI 1006 steel

This study investigated a conversion coating based on hexafluorozirconic acid solution on cold-rolled (AISI 1006) steel sheets, in situ, at different pH values and immersion times. Electrochemical characterization was carried out by electrochemical impedance spectroscopy (EIS) with hexafluorozirconic acid bath as the electrolyte. Laser scanning confocal microscopy (LSCM) was used to evaluate the morphology of the coating in situ, i.e., during the coating formation. According to the results, the polarization resistance (Rp) of the conversion coating is affected by the immersion time and by the pH of the conversion bath. The electrochemical analyzes point out conversion baths at pH between 3.5 and 4.5 and immersion times from 600 to 900 s as optimal operating conditions, achieving an average polarization resistance of 713 ± 107 Ω cm2

Synthesis of Yttria Stabilized Zirconia by sol–gel route: Influence of experimental parameters and large scale production

This paper develops an advance in the field of new synthesis techniques for functional materials like Yttria Stabilized Zirconia (YSZ) used as sensors, thermal barriers or electrolytes for high-temperature fuel cells. In recent years, sol–gel routes were developed to prepare, by suitable chemical modifications, submicronic based materials with a controlled morphology, which conventional solid state chemistry paths are unable to provide. Wet chemistry methods provide interesting alternative routes because mixing of species occurs on the atomic scale. In this paper, ultrafine powders were prepared by a novel wet chemistry method based on the sol–gel process. One of the advantages of this method is to decrease the crystallization temperature in comparison to the conventional ones, allowing the synthesis of reactive powders with nanometric particles size. In this study, several processing parameters have been investigated (the hydrolysis ratio, the concentration of metallic precursors in the sol and the role of organic compounds and additives). Pure phases of YSZ were obtained and the characteristics of these powders investigated (crystallographic study, morphology, phase composition, etc.). Also, our optimised synthesis was applied to large scale elaboration by increasing the quantity of precursors. This study underlines the interest of the sol–gel process both to control the morphology of oxides and to prepare large amounts of high purity powders for an eventual industrialization process

The influence of surface condition on the electrochemical properties of ASTM F138 steel for biomedical applications

The aim of this paper was to determine the influence of machining parameters on the surface layer, and consequently on the electrochemical properties, of ASTM F138 austenitic stainless steels. Eight different surface conditions were generated in cylindrical samples by turning and polishing. The surface was characterized by surface roughness Ra and Rt, Vickers microhardness and microstructural characteristics. Cyclic voltammetric tests were performed to evaluate the potential of repassivation and pitting. The surfaces were analyzed by Scanning Electron Microscopy after the electrochemical tests were performed. The cutting parameters were identified to have a significant influence, and the feed rate was as influential as the depth of cut. The use of polishing alone is not sufficient to ensure that a surface has good surface integrity. Even with the polishing application, usually used to produce prostheses, a significant reduction in corrosion resistance occurs if care is not taken to minimize surface machining damage. Corrosion resistance is lower and pitting nucleation is higher in the samples with no polishing and with more severe machining parameters. The tests indicated that softer machining parameters can contribute to an increase in the life of implantable components, reducing the probability of localized corrosion, as well as improving the mechanical properties of prostheses