Avaliação das condições de precipitação do azul da Prússia sobre pó de grafite visando o desenvolvimento de eletrodos de pasta de carbono para a quantificação de nitrito

An amperometric FIA method for nitrite quantification based on nitrite electroreduction and employing a carbon paste electrode (CPE) chemically modified with iron hexacyanoferrate (HCF) as an amperometric detector was developed. The influence of experimental conditions on the preparation of the electrode materials was evaluated and the materials obtained in each study were used for the development of modified electrodes. The electrochemical sensors were prepared by a fast, simple, and inexpensive procedure, and the long-term performance of the electrodes were quite satisfactory as the stability was maintained over one year. HCF was an effective redox mediator for nitrite electroreduction in acidic media, allowing nitrite detection at +0.2 V vs. Ag/AgClsat, which is a potential free of possible interfering species that are normally present in food and water samples. The electrochemical cell used in the FIA system was similar to a batch injection analysis cell, enabling recirculation of the carrier solution. This is an attractive feature because it allows the use of a high flow rate (6 mL min-1) leading to high sensitivity and analysis speed, while keeping reagent consumption low. The proposed method had a detection limit of 9 μmol L-1 and was successfully employed for nitrite quantification in spiked water and sausage samples. The obtained results were in good agreement with those provided by the spectrophotometric official method. At a 95 % confidence level it was not observed statistical differences neither in nitrite content nor in the precision provided by both methods. The experimental conditions for the synthesis of HCF were optimized and the best electrode material was prepared by mixing FeCl3, K4[Fe(CN)6] and carbon powder subjected to an acid and thermal treatment (400 ºC), followed by ultrasonic agitation at 4 °C. This material was used to construct an electrode with improved analytical performance to reduce nitrite, which presented greater stability compared to HCF film electrodeposited on the EPC, showing that the preparation procedure of the electrode material is an effective strategy for the development of HCF modified electrodes.

Retificação plana tangencial dos ferros fundidos nodular, vermicular e cinzento em várias condições de corte

In a scenario of increasing competitiveness of the global industrial sector and with a consumer market increasingly demanding, there is an increased demand for new materials and, consequently, possibilities to explore new research and technological advances towards the development of new manufacturing methods or the improvement of existing technologies. In the case of cast irons, new grades of them have been developed so that their mechanical properties have been improved, making them more competitive with steel, expanding the applications and thus represents great economic gain for metallurgy and manufacturing sectors. This increases the interest and creates new opportunities to study these materials and identify how they respond in terms of the surface integrity, tool wear, cutting forces, among others, when machined by grinding operation. In this context, due to the lack of results from grinding of cast irons and studies comparing grindability among several grades of cast irons found in the literature, this work aims to generate scientific and technological contribution to the metallurgical and metal working sector through roughness results (Ra and Rz parameters) and evaluation and analysis of the subsurface integrity of three cast iron grades (gray, compacted graphite and nodular). The machining trials were performed on a surface grinding machine with silicon carbide grinding wheel at different cutting conditions. The input variables were the radial depth of cut (15 and 30 μm), worktable speed, vw (5 and 10 m/min) and the abrasive grain size of the grinding wheel. The results showed that surface roughness increased with the radial depth of cut for all materials tested; and the lowest values were obtained for gray cast iron. Also, roughness was sensitive to variation of worktable speed and the lowest values were obtained after machining with vw = 5 m/min. With respect to the abrasive grain size, as it decreased the roughness values increased to gray and nodular cast iron grades. Furthermore, grinding burns marks were observed on the surfaces of nodular cast iron and compacted graphite iron grades after grinding the smallest grain size, contrary to what is usually reported in literature. However, no evidence of severe thermal damages below the machined surfaces of all cast iron grades was observed after analyzing the results of hardness and the SEM micrograph images.