Determinação voltamétrica de zinco empregando eletrodos quimicamente modificados com bismuto

This dissertation presents the development of voltammetric methods to zinc determination in multivitamin commercial samples, talc, and art materials for painting (soft pastel) combining an alkaline extraction with 1.0 mol L-1 NaOH aqueous solution and bismuth modified electrodes. Two electrodes were used to zinc quantification in the samples, bismuth film electrode (BiFE) plated in situ onto glassy carbon and carbon paste electrode chemically modified with strongly acidic ion exchange resin Amberlite® IR 120 and bismuth nanostructures (EPCAmbBi). It was verified that the best concentration of Bi3+ for Bi film deposition onto glassy carbon was 4.0 μmol L-1 using an 0.1 mol L-1 acetate buffer aqueous solution (pH = 4.5) as supporting electrolyte. The best condition to formation of Bi nanostructures in the EPC modified with 10 % Amberlite® IR 120 was the use of 30 s to pre-concentration (open circuit) in 0.5 mmol L-1 Bi3+ aqueous solution (pH 5.5) prepared with supporting electrolyte solution. The obtained analytical curve for Zn2+ using BiFE presented linear range from 0.5 to 5.0 μmol L-1, the limit of detection (LD) was 41 nmol L-1. For EPCAmbBi only one linear range was observed for the analytical curve varying the Zn2+ concentration from 0.05 to 8.2 μmol L-1, LD obtained in this curve it was equal to 10 nmol L-1. The EPCAmbBi presented the most intense and sharp anodic stripping peaks for Zn2+ presenting, therefore, a better voltammetric profile, with sensitivity higher than obtained with the BiFE. Moreover, the EPCAmbBi presented a LD lower than that obtained with the BiFE. Alkaline extraction was an efficient sample pretreatment to extract Zn2+ from solid samples, besides that, this procedure was less susceptible to interferences from Cu2+, since it remains at extracting vessel as insoluble Cu(OH)2. The combination of alkaline extraction with the EPCAmbBi is a simple, fast, efficient and low cost for the zinc determination in pharmaceutical formulations and art materials for painting (soft pastel) samples, which can be employed as a low-cost alternative method to the atomic absorption spectroscopy.

Influência da utilização do fluido de corte com adição de grafeno na temperatura de usinagem e formação de rebarba no processo de micro fresamento

As time passed, humanity needed the development of new materials used in various activities. High strength materials such as titanium and Inconel for example, had been studied because they are widely used for implants in biomedicine, as well as their use in aerospace and automotive industries. Because of its thermal and mechanical properties, these materials are considered difficult to machine, promoting a rapid wear of cutting tools, primarily caused by the high temperatures in machining. With the development of new materials has emerged the need of developing new manufacturing processes. One of today’s innovative processes is the micro-manufacturing. Being a process with a defined cutting tool geometry, burr formation is a constant and undesirable phenomenon formed during the machininig process. Being detrimental to the manufacturing process, overspending deburring operations are constantly employed leading to increase the aggregate cost to the manufactured material. Assembly components are also impaired if there is no control of the burr, with consequences including the disposal of components due to the occurence of this phenomenon. This paper presents the study of micro-milling Inconel 718, investigating influential parameters in the formation of burrs in order to minimize the occurrence of this phenome non. Different feed rates per tooth and cutting speed are evaluated, and different cutting fluids with different methods of applying the fluid. Adding graphene to cutting fluids was considered as a variable to be investigated, which is considered an excellent solid lubricant, in addition to increasing the thermal conductivity of the cooling solution (AZIMI; MOZAF FARI, 2015). The micro-milling temperature was evaluated in the present work. It was observed a new phenomenon that causes the machined surface temperature decreases below room temperature when using the solution water + oil. This phenomenon is explained in further chapters. In order to unravel this phenomenon, a new test was proposed and, from this test, it can be concluded, comparatively, which cutting fluid has a better cooling property.Using cutting fluid with different thermal properties has shown influence when analy zing burr formation and reducing machining temperature.