Aplicabilidade da voltametria de pulso diferencial na quantificação de ácido fólico e ácido oxálico: um método comparativo

The development of more selective and sensitive analytical methods is of great importance in different areas of knowledge, covering, for example, food, biotechnological, environmental and pharmaceutical sectors. The study aimed to employ the technique electroanalytical differential pulse voltammetry (DPV) as an innovative and promising alternative for identification and quantification of organic compounds. The organic compounds were investigated in this study oxalic acid (OA) and folic acid (FA). The electrochemical oxidation of oxalic acid has been extensively studied as a model reaction in the boundary between the organic and inorganic electrochemistry. Since the AF, an essential vitamin for cell multiplication in all tissues, which is essential for DNA synthesis. The AF has been investigated using analytical techniques, liquid chromatography and molecular absorption spectrophotometry. The results obtained during the experimental procedure indicated that the process of electrochemical oxidation of oxalic acid is strongly dependent on the nature of the anode material and the oxidation mechanism, which affects their detection. Efficient removal was observed in Ti/PbO2 anodes, graphite, BDD and Pt 90, 85, 80 and 78% respectively. It was also shown that the DPV employing glassy carbon electrode offers a fast, simple, reliable and economical way to determine the AO during the process of electrochemical oxidation. Furthermore, electroanalytical methods are more expensive than commonly used chromatographic analysis and other instrumental methods involving toxic reagents and higher cost. Compared with the classical method of titration and DPV could be a good fit, confidence intervals and detection limits confirming the applicability of electroanalytical technique for monitoring the degradation of oxalic acid. For the study of AF was investigated the electrocatalytic activity of the carbon paste electrode for identification and quantification in pharmaceutical formulations by applying the DPV. The results obtained during the experimental procedure showed an irreversible oxidation peak at 9.1 V characteristic of FA. The carbon paste sensor showed low detection limit of 5.683×10−8 mol L-1 reducing matrix effects. The spectrophotometric analysis showed lower concentrations of HF compared with those obtained by HPLC and DPV. The levels of AF were obtained according to the methodology proposed by the Brazilian Pharmacopoeia. The electroanalytical method (DPV) proposed is cheaper than GC analysis commonly used by the pharmaceutical industry. The results demonstrated the potential of these electroanalytical techniques for future applications in environmental, chemical and biological sensors

Adsorção de Mn (II) e Zn (II) em soluções aquosas usando perlita expandida revestida com quitosana

In this work, chitosan was used as a coating of pure perlite in order to increase the accessibility of the groups OH- e NH2+the adsorptionof ions Mn2+ e Zn2+.The characterization results of the expanded perlite classified as microporous and whose surface area 3,176 m2 g-1after the change resulted in 4,664 m2g-1.From the thermogravimetry(TG) it was found that the percentage of coating was34,3%.The infrared analysis can prove the presence of groups Si-OH, Si-O e Al-O-Siresulting from the perlite and C=O, NH2and OH characterization of chitosan. The experiments on experiments on the adsorption of Mn and Zn were performed in the concentration range of10 a 50 mgL-1and the adsorption capacity inpH 5,8 e 5,2 was 19,49 and 23,09 mgg-1to 25 oC,respectively.The adsorption data were best fitted to Langmuir adsorption model to Langmuir adsorption model for both metalionsisindicative of monolayer adsorption. The kinetics of adsorption were calculated from the equation of Lagergren fitting the model pseudo-second-order for all initial concentrations, suggesting that adsorption of ions Mn2+ and Zn2+ follows the kinetics of pseudo-second-order and whose constant Speedk2(g/mg.min) are 0,105 e 3,98 and capacity and maximum removal qe 4,326 e 3,348,respectively.In this study we used a square wave voltammetry cathodic stripping voltammetry to quantify the adsorbed ions, and the working electrode glassy carbon, reference electrode silver / silver chloride and a platinum auxiliary electrode. The attainment of the peaks corresponding to ions Mn2+ and Zn2+ was evaluated in and electrochemical cell with a capacity of 30 mL using a buffer system (Na2HPO4/NaH2PO4)at pH 4 and was adjusted with solutionsH3PO4 0,1molL-1and NaOH 0,1 molL-1and addition of the analyte has been a cathodic peak in- 0,873 Vand detection limit of2,55x10-6molL-1para Zn.The dough used for obtaining the adsorption isotherm was 150 mg and reached in 120 min time of equilibrium for both metal ions.The maximum adsorption for 120 min with Mn concentration 20 mgL-1 and Zn 10 mgL-1,was91, 09 e 94, 34%, respectively

Aplicação da técnica eletroanalítica de pulso diferencial usando o eletrodo de carbono vítreo modificado com cisteína para monitorar a degradação eletroquímica de ácido oxálico

In this paper, the technique of differential pulse voltammetry (DPV) has been studied for monitoring the concentration of oxalic acid (OA) during their electrochemical oxidation (EO) in acidic medium using platinum anode supported on titanium (Ti / Pt). The DPV was standardized and optimized using a glassy carbon electrode modified with cysteine. The modification with cysteine was developed electrochemically, forming a polymeric film on the surface of the glassy carbon electrode. The formation of the polymer film was confirmed by analysis of scanning electron microscope and atomic force microscope, confirming the modification of the electrode. The electrochemical degradation was developed using different current densities 10, 20 30 and 40 mA cm -2 electrode with Ti / Pt observing the degradation of oxalic acid, and monitored using the method of KMnO4 titration. However, the analyzes with DPV showed the same behavior elimination of oxalic acid titration. Compared with the titration method classical observed and DPV could be a good fit, confidence limits of detection and confirming the applicability of the technique electroanalytical for monitoring the degradation of oxalic acid

Degradação eletroquímica de benzeno, tolueno e xileno via oxidação eletroquímica utilizando eletrodo Ti/Pt

This work is directed to the treatment of organic compounds present in produced water from oil using electrochemical technology. The water produced is a residue of the petroleum industry are difficult to treat , since this corresponds to 98 % effluent from the effluent generated in the exploration of oil and contains various compounds such as volatile hydrocarbons (benzene, toluene, ethylbenzene and xylene), polycyclic aromatic hydrocarbons (PAHs), phenols, carboxylic acids and inorganic compounds. There are several types of treatment methodologies that residue being studied, among which are the biological processes, advanced oxidation processes (AOPs), such as electrochemical treatments electrooxidation, electrocoagulation, electrocoagulation and eletroredution. The electrochemical method is a method of little environmental impact because instead of chemical reagents uses electron through reactions of oxide-reducing transforms toxic substances into substances with less environmental impact. Thus, this paper aims to study the electrochemical behavior and elimination of the BTX (benzene, toluene and xylene) using electrode of Ti/Pt. For the experiment an electrochemical batch system consists of a continuous source, anode Ti/Pt was used, applying three densities of current (1 mA/cm2, 2,5 mA/cm2 and 5 mA/cm2). The synthetic wastewater was prepared by a solution of benzene, toluene and xylene with a concentration of 5 ppm, to evaluate the electrochemical behavior by cyclic voltammetry and polarization curves, even before assessing the removal of these compounds in solution by electrochemical oxidation. The behavior of each of the compounds was evaluated by the use of electrochemical techniques indicate that each of the compounds when evaluated by cyclic voltammetry showed partial oxidation behavior via adsorption to the surface of the Ti/Pt electrode. The adsorption of each of the present compounds depends on the solution concentration but there is the strong adsorption of xylene. However, the removal was confirmed by UV-Vis, and analysis of total organic carbon (TOC), which showed a percentage of partial oxidation (19,8 % - 99,1 % TOC removed), confirming the electrochemical behavior already observed in voltammetry and cyclic polarization curves

Estudo da participação das espécies fortemente oxidantes produzidas durante a oxidação eletroquímica de corantes usando eletrodo de diamante dopado com boro: função das propriedades eletroquímicas do eletrodo e condições experimentais

The textile industry is one of the most polluting in the world (AHMEDCHEKKAT et al. 2011), generating wastewater with high organic loading. Among the pollutants present in these effluents are dyes, substances with complex structures, toxic and carcinogenic characteristics, besides having a strong staining. Improper disposal of these substances to the environment, without performing a pre-treatment can cause major environmental impacts. The objective this thesis to use a technique of electrochemical oxidation of boron doped diamond anode, BDD, for the treatment of a synthetic dye and a textile real effluent. In addition to studying the behavior of different electrolytes (HClO4, H3PO4, NaCl and Na2SO4) and current densities (15, 60, 90 and 120 mA.cm-2 ), and compare the methods with Rhodamine B (RhB) photolysis, electrolysis and photoelectrocatalytic using H3PO4 and Na2SO4. Electrochemical oxidation studies were performed in different ratio sp3 /sp2 of BDD with solution of RhB. To achieve these objectives, analysis of pH, conductivity, UV-visible, TOC, HPLC and GC-MS were developed. Based on the results with the Rhodamine B, it was observed that in all cases occurred at mineralization, independent of electrolyte and current density, but these parameters affect the speed and efficiency of mineralization. The radiation of light was favorable during the electrolysis of RhB with phosphate and sulfate. Regarding the oxidation in BDD anode with different ratio sp3 /sp2 (165, 176, 206, 220, 262 e 329), with lower carbon-sp3 had a longer favoring the electrochemical conversion of RhB, instead of combustion. The greater the carbon content on the anodes BDD took the biggest favor of direct electrochemical oxidation

Regulação da mobilização de lipídios e proteinas por hormônios, fontes de carbono e nitrogênio durante o crescimento pos-germinativo em girassol

The mobilization of food reserves in storage tissues and allocation of their hydrolysis products in the growing axis are critical processes for the establishment of seedlings after germination. Therefore, it is crucial for mobilization of reserves to be synchronized with the growing axis, so that photosynthetic activity can be started before depletion of reserves. For this, integrative approaches involving different reserves, different hydrolysis products and interaction between storage and growing axis tissues, either through hormones or metabolites with signaling role, can contribute greatly to the elucidation of the regulation mechanisms for reserve mobilization. In this study, was hypothesized that hormones and metabolites have different actions on reserve mobilization, and there must be a crossed effect of sugars on the mobilization of proteins and amino acids on lipids and starch mobilization in sunflower seedlings. This study was conducted with seeds of sunflower (Helianthus annuus L.) hybrid Helio 253 using in vitro culture system. Seeds were germinated on Germitest® paper and grown on agar-water 4 g/L without addition of nutrients during 9 days after imbibition (DAI) for growth curve. To verify the effect of metabolites and hormones, seedlings were transferred in the 2nd DAI to agar-water 4 g/L supplemented with increasing concentrations of sucrose or L-glutamine, abscisic acid, gibberellic acid or indolebutyric acid. The results of this study confirm that the mobilization of lipids and storage proteins occurs in a coordinated manner during post-germination growth in sunflower, corroborating the hypothesis that the application of external carbon (sucrose) and nitrogen (L-glutamine) sources can delay the mobilization of these reserves in a crossed way. Moreover, considering the changes in the patterns of reserve mobilization and partition of their products in seedlings treated with different growth regulators, it is evident that the effects of metabolites and hormones must involve, at least in part, distinct mechanisms of action

Análise e avaliação dos elementos de penetração no solo de equipamentos rodoviários após revestimento

The main objective is to analyze the abrasive wear resistance to the low stress of the elements that make up the organs of road machinery that are exposed directly to contact with abrasives. These samples were analyzed after these elements are coated superficially by the process of welding electrode coated with (SAER) and the manual process of coating type LVOF thermal spraying. As well, is to provide suggestions for a better recovery and return of these elements, which are reducing costs and avoiding downtime in the fronts of service. The samples were made from a substrate of carbon ABNT 1045 tempered steel, following the same specifications and composition of metals and alloys of constituents was followed the standard governing the dimensions of these samples and in accordance with the corresponding size. The results were evaluated by testing the hardness, abrasion resistance to wear by the low stress and the loss of volume involving the microstructure of coatings analyzed

Estudos de Durabilidade Frente ao Ataque Ácido de Compósitos Portland-Polímero para Cimentação de Poços de Petróleo

Portland-polymers composites are promising candidates to be used as cementing material in Northeastern oil wells of Brazil containing heavy oils submitted to steam injection. In this way, it is necessary to evaluate its degradation in the commonly acidizind agents. In addition, to identify how aggressive are the different hostile environments it is an important contribution on the decision of the acidic systems to be used in. It was investigated the performance of the Portland-polymer composites using powdered polyurethane, aqueous polyurethane, rubber tire residues and a biopolymer, those were reinforced with polished carbon steel SAE 1045 to make the electrochemical measurements. HCl 15,0 %, HCl 6,0 % + HF 1,5 % (soft mud acid), HCl 12,0 % + HF 3,0 % (regular mud acid) and HAc 10 % + HF 1,5 % were used as degrading environment and electrolytes. The more aggressive acid solution to the plain Portland hardened cement paste was the regular mud acid, that showed loss of weight around 23.0 %, followed by the soft mud acid, the showed 11.0 %, 15.0 % HCl with 7,0 % and, at last the 10.0 % HAc plus HF 1.5 % with just 1.0 %. The powdered polyurethane-composite and the aqueous polyurethane one showed larger durability, with reduction around 87.0 % on the loss of weight in regular mud acid. The acid attack is superficial and it occurs as an action layer, where the degraded layer is responsible for the decrease on the kinetic of the degrading process. This behavior can be seen mainly on the Portland- aqueous polyurethane composite, because the degraded layer is impregnated with chemically modified polymer. The fact of the acid attack does not have influence on the compressive strength or fratography of the samples, in a general way, confirms that theory. The mechanism of the efficiency of the Portland-polymers composites subjected to acid attack is due to decreased porosity and permeability related with the plain Portland paste, minor quantity of Ca+2, element preferentially leached to the acidic solution, wave effect and to substitute part of the degrading bulk for the polymeric one. The electrolyte HAc 10 % + HF 1,5 % was the least aggressive one to the external corrosion of the casing, showing open circuit potentials around +250 mV compared to -130 mV to the simulated pore solution to the first 24 hours immersion. This behavior has been performed for two months at least. Similar corrosion rates were showed between both of the electrolytes, around 0.01 μA.cm-2. Total impedance values, insipient arcs and big polarization resistance capacitive arcs on the Nyquist plots, indicating passivity process, confirm its efficiency. In this way, Portlandpolymers composites are possible solutions to be succeed applied to oilwell cementing concomitant submitted to steam injection and acidizing operation and the HAc 10,0 % + HF 1,5 % is the less aggressive solution to the external corrosion of the casing

Avaliação de inibidores verdes microemulsionados na inibição à corrosão do aço carbono AISI 1020

In general, among the corrosion inhibitors surfactants are the most commonly used compounds, because they are significantly effective by forming protective films on anodic and cathodic areas. In this study, microemulsions containing he biodegradable saponified coconut oil as surfactant (SME-OCS) was used as green corrosion inhibitors. With this purpose, methanolic extracts of Ixora coccinea Linn (IC) and a polar fraction rich in alkaloids (FA) obtained from Croton cajucara Benth solubilized in the SME-OCS system were examined in the presence of AISI 1020 carbon steel, in saline solution (NaCl 3,5 %). The efficiency of corrosion inhibition of IC and FA were evaluated in the following microemulsions: SME-OCS-IC and SME-OCS-FA. The microemulsion system SME-OCS in the presence and absence of IC and FA was assessed by measurements of weight loss and the electrochemical method of polarization resistance, with variation in the concentration of IC and FA (50 - 400 ppm), showing significant results of corrosion inhibition (83,6 % SME-OCS; 92,2 % SME-OCS-FA; and 95,3 % SME-OCS-IC)

Utilização de matérias primas vegetais para aplicabilidade como inibidores de corrosão

In the search for products that act as corrosion inhibitors and do not cause environmental, impact the use of plant extracts as corrosion inhibitors is becoming a promising alternative. In this work the efficiency of polar extracts (ethanol extracts) obtained from the plants Anacardium occidentale Linn (AO) and Phyllantus amarus Schum. & Thonn (PA) as corrosion inhibitors were evaluated in different concentrations. For that AO and PA extracts were solubilized in the microemulsion systems (SME) containing saponified coconut oil as surfactant (SME -OCS and SME-OCS-1) in saline (NaCl 3,5 %) solution, which was also used as electrolyte. Both SME-OCS and SME-OCS-1 were characterized by surface tension and viscosity methods showing a Newtonian fluid behavior. The SME-OCS and SME-OCS-1 systems satisfactorily solubilized the polar extracts AO and PA with measurements carried out by ultraviolet spectroscopy. The measurements of corrosion inhibition efficiencies were performed by the electrochemical linear polarization resistance (LPR) technique as well as weight loss, on the surface of AISI 1020 carbon steel. The maximum corrosion inhibition efficiencies were determined by extrapolation of Tafel plots, showing the following values: 95,6 % for the system SME-OCS-AO, 98,9 % for the system SME-OCS-AO-1 and 93,4 % for the system SME-OCS-PA

Desenvolvimento de um sistema misto de pasta à base de geopolímero e cimento portland para correção de perda de circulação

The materials engineering includes processes and products involving several areas of engineering, allowing them to prepare materials that fulfill the needs of various new products. In this case, this work aims to study a system composed of cement paste and geopolymers, which can contribute to solving an engineering problem that directly involves the exploitation of oil wells subject to loss of circulation. To correct it, has been already proposed the use of granular materials, fibers, reducing the drilling fluid or cement paste density and even surface and downhole mixed systems. In this work, we proposed the development of a slurry mixed system, the first was a cement-based slurry and the second a geopolymer-based slurry. The cement-based slurry was formulated with low density and extenders, 12.0 ppg (1.438 g/cm ³), showing great thixotropic characteristics. It was added nano silica at concentrations of 0.5, 1.0 and 1.5 gps (66.88, 133.76 and 200.64 L/m3) and CaCl2 at concentrations of 0.5, 1, 0 and 1.5%. The second system is a geopolymer-based paste formulated from molar ratios of 3.5 (nSiO2/nAl2O3), 0.27 (nK2O/nSiO2), 1.07 (nK2O/nAl2O3) and 13.99 (nH2O/nK2O). Finally, we performed a mixture of these two systems, for their application for correction of circulation lost. To characterize the raw materials, XRD, XRF, FTIR analysis and titration were performed. The both systems were characterized in tests based on API RP10B. Compressive strength tests were conducted after curing for 24 hours, 7 and 28 days at 58 °C on the cement-based system and the geopolymer-based system. From the mixtures have been performed mixability tests and micro structural characterizations (XRD, SEM and TG). The results showed that the nano silica, when combined with CaCl2 modified the rheological properties of the cement slurry and from the concentration of 1.5 gpc (200.64 L / m³) it was possible to obtain stable systems. The system mixture caused a change in the microstructure of the material by favoring the rate of geopolymer formation to hinder the C3S phase hydration, thus, the production of CSH phases and Portlandite were harmed. Through the mixability tests it can be concluded that the system, due to reduced setting time of the mixture, can be applied to plug lost circulation zones when mixed downhole

Estudo comparativo de pás para aerogeradores de grande porte fabricadas em materiais compósitos reforçadas com fibra de carbono ou fibra de vidro

The research and development of wind turbine blades are essential to keep pace with worldwide growth in the renewable energy sector. Although currently blades are typically produced using glass fiber reinforced composite materials, the tendency for larger size blades, particularly for offshore applications, has increased the interest on carbon fiber reinforced composites because of the potential for increased stiffness and weight reduction. In this study a model of blade designed for large generators (5 MW) was studied on a small scale. A numerical simulation was performed to determine the aerodynamic loading using a Computational Fluid Dynamics (CFD) software. Two blades were then designed and manufactured using epoxy matrix composites: one reinforced with glass fibers and the other with carbon fibers. For the structural calculations, maximum stress failure criterion was adopted. The blades were manufactured by Vacuum Assisted Resin Transfer Molding (VARTM), typical for this type of component. A weight comparison of the two blades was performed and the weight of the carbon fiber blade was approximately 45% of the weight of the fiberglass reinforced blade. Static bending tests were carried out on the blades for various percentages of the design load and deflections measurements were compared with the values obtained from finite element simulations. A good agreement was observed between the measured and calculated deflections. In summary, the results of this study confirm that the low density combined with high mechanical properties of carbon fibers are particularly attractive for the production of large size wind turbine blades

Estudo do resíduo fosfogesso na formulação de uma pasta para revestimento interno de edifícios

Universidade Federal do Rio Grande do Norte

Avaliação da correlação entre os parâmetros, carbono orgânico total e elementos tóxicos, em solo de um posto de serviço e revenda de combustíveis

Today a major responsibility for the contamination of soil and groundwater and surface water are establishments known as gas stations of fuel which has attracted increasing attention from both the general population as the state agencies of environmental control due to leaks in storage tanks and mainly to disruption of pipe corrosion of tanks and pumping. Other services, like oil changes and car wash are also causes for concern in this type of establishment. These leaks can cause or waste produced, and the contamination of aquifers, serious health problems and public safety, since most of these stations located in urban areas. Based on this, the work was to evaluate soil contamination of a particular service station and fuel sales in the city of Natal, through the quantification of heavy metals like Cd, Cu, Cr, Ni, Pb, Zn of total organic carbon (TOC) and organic matter using different techniques such as optical emission spectrometry with inductively coupled plasma source (ICP OES), Total Organic Carbon analyzer and gravimetric analysis respectively. And also to characterize the soil through particle size analysis. Samples were taken in 21 georeferenced points and collected in the same period. The soils sampled in sampling stations P3, P5, P6, P10, P11, P12, P13, P14, P15, P17, P18 and P20 showed the smallest size fractions ranging from fine sand to medium sand. The other study sites ranged from fine sand to medium sand, except the point P8 showed that only the type size medium sand and P19, indicating a particle size of the coarse type. The small correlation of organic matter with the elements studied in this work suggests that these are not of anthropogenic origin but geochemical support

Tratamento eletroquímico de efluente proveniente de caixas separadoras de água e óleo de postos revendedores de combustíveis

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior