This paper presents a proposal for using recycled graphite electrodes obtained from exhausted commercial 1.5 V batteries and its application in electroanalysis. The electrode could be prepared by the students and applied in the simple didactic experiments suggested, such as determination of active electrode area, cyclic voltammetry and useful potential range (also called "potential window"), demonstration and effect of scan rate on cyclic voltammograms. The possibility of using the graphite electrode in quantitative analysis was also demonstrated using the ferricyanide/ferrocyanide reversible redox couple ([Fe(CN)6]3-/[Fe(CN)6]4-) as an electrochemical probe by the dependence of peak current with the analyte concentration and flow injection analysis with amperometric detection.

Alkaline salts of the palmitic acid were synthesized and characterized from aqueous and ethanolic medium. The salts were characterized by elemental analysis (EA) and infrared spectroscopy (IR). EA and IR, being its synthesis comproved, also characterized the ethyl palmitate. All the salts and the ester were submitted to thermal analysis using thermogravimetry (TG), and differential thermal analysis (DTA) in the temperature ranging from room to 700 ºC under air dynamic atmosphere. Differential scanning calorimetry (DSC) measurements were taken from -90 ºC up to temperatures close to the starting of the decomposition temperature, determined by thermogravimetry, using heating and cooling cycles.

Thermoanalytical behavior of sodium and potassium salts of pyrrolidinedithiocarbamate (pyr), piperidineditiocarbamate (pip), morpholinedithiocarbamate (mor), hexametileneiminedithiocarbamate (hex), were investigated. In a first step the salts were synthesized and characterized by infrared spectroscopy (FTIR), ¹H and 13C nuclear magnetic resonance (NMR) and elementar analysis. Finally, thermal analytical (TG/DTG and DSC) studies were performed in order to evaluate the thermal stability, as well as the pathways of the thermal decomposition based in the intermediate and final decomposition products.

Considering the attraction of the students' attention by the changes in the colors of vegetable crude extracts caused by the variation of the pH of the medium, the use of these different colors in order to demonstrate principles of spectrophotometric acid-base titrations using the crude extracts as indicators is proposed. The experimental setup consisted of a simple spectrophotometer, a homemade flow cell and a pump to propel the fluids along the system. Students should be stimulated to choose the best wavelength to monitor the changes in color during the titration. Since the pH of the equivalence point depends on the system titrated, the wavelength must be properly chosen to follow these changes, demonstrating the importance of the correct choice of the indicator. When compared with the potentiometric results, errors as low as 2% could be found using Rhododendron simsii (azalea) or Tibouchina granulosa (Glory tree, quaresmeira) as sources of the crude extracts.

Aspects of visible spectrophotometry can be presented to students using simple experiments in which the color of the crude extract of Macroptilium lathyroides (L.) Urb. is bleached in the presence of nitrite ions in acidic medium. The dependence of the absorption intensity with time, the reaction completeness and the Beer law can be demonstrated. Quantitative results for mineral water samples "contaminated" with nitrite ions were obtained from a method based on the Griess reaction and a procedure based on the bleaching reaction between the crude extract and NO2- ions. Both the Griess and the bleaching reactions were found to be time dependent. Recoveries of about 100 - 104% were obtained with these procedures. The use of natural dyes attracted students' interest enhancing the teaching process. Experiments performed by the teaching staff suggested that the proposed methodology can be performed in a 4 h class, with relative errors ranging from 0.19 to 1.86% in relation to the Griess method.

The construction and analytical evaluation of a coated graphite-epoxy electrode sensitive to the zinc-1,10-phenantroline complex based on the [Zn(fen)3][tetrakis(4-chlorophenyl)borate]2 incorporated into a poly(vinylchloride) (PVC) matrix are described. A thin membrane film of this ion-pair, dibutylphthalate (DBPh) and PVC were deposited directly onto an electrically conductive graphite-epoxy support located inside a Perspex® tube. The best PVC polymeric membrane contains 65% (m/m) DBPh, 30% (m/m) PVC and 5% (m/m) of the ion-pair. This electrode shows a response of 19.5 mV dec-1 over the zinc(II) concentration range of 1.0 x 10-5 to 1.0 x 10-3 mol L-1 in 1,10-phenantroline medium, at pH 6.0. The response time was less than 20 seconds and the lifetime of this electrode was more than four months (over 1200 determinations by each polymeric membrane). It was successfully used as an indicator electrode in the potentiometric precipitation titration of zinc(II) ions.

In this work, a spectrophotometric flow injection analysis system using a crude extract of avocado (Persea americana) as a source of polyphenol oxidase to dopamine determination was developed. The substrates and enzyme concentrations from 2.4x10-7 to 5.3x10-4 mol L-1 and 28 to 332 units mL-1 were evaluated, respectively. In addition, the FIA parameters such as sample loop (50 to 500 µL), flow rate (1.4 to 4.3 mL min-1) and reactor length (100 to 500 cm) were also evaluated in a 0.1 mol L-1 phosphate buffer solution (pH 7.0). Dopamine solution concentrations were determined using 277 units mL-1 enzyme solution, 400 mL enzyme loop, 375 µL sample loop, 2.2 mL min-1 flow rate and a reactor of 350 cm. The analytical curve showed a linearity from 5.3x10-5 to 5.3x10-4 mol L-1 dopamine with a detection limit of 1.3x10-5 mol L-1. The analytical frequency was 46 h-1 and the RSD lower than 0.5% for 5.3x10-4 mol L-1 dopamine solution (n=10). A paired t-test showed that all results obtained for dopamine in commercial formulations using the proposed flow injection procedure and a spectrophotometric procedure agree at the 95% confidence level.

No presente trabalho, foi desenvolvido um eletrodo de PbO2 eletrodepositado sobre grafite a partir do eletrólito metanosulfonato de chumbo-ácido metanosulfônico contendo o agente tensoativo brometo de cetiltrimetilamônio (BCTA). Foram avaliadas a resposta potenciométrica do eletrodo de PbO2 como sensor à íons Pb2+ e SO4(2-), em pH e força iônica constante. A aplicação deste eletrodo em titulações potenciométricas de precipitação em meio hidro-etanólico também foi investigada. Os resultados demonstraram que o eletrodo de PbO2 eletrodepositado pode ser utilizado como sensor potenciométrico alternativo à íons Pb(II) apresentando uma linearidade na faixa de concentração de 3,98x10-4 a 3,09x10-2 mol L-1 em meio de íons nitrato com limite de detecção de (4,98 ± 0,11)x10-4 mol L-1. Para íons sulfato o eletrodo de PbO2 não responde diretamente porém, estes íons podem ser dosados indiretamente por titulação potenciométrica com solução padrão de Pb(II), em meio ácido, em uma mistura 1:1 (v/v) de etanol-água, com boa definição dos volumes de equivalência. A repetitividade dos potenciais e dos volumes de equivalência obtidos em amostras de concentração milimolar em sulfato, indicam a viabilidade deste eletrodo na dosagem de íons sulfato.

The development of a PbO2 electrodeposited in a graphite substrate electrode and evaluation of its potenciometric response as a sensor for Pb2+ and SO4(2-) ions, at constant pH and ionic strength is described. The electrode was applicated in the potenciometric titration in precipitation reaction of Pb2+ with SO4(2-) in hydro-ethanolic medium. The results showed that the PbO2 electrodeposited electrode is useful as a potenciometric sensor to the Pb(II) ions presenting a linear response range between 3,98x10-4 a 3,09x10-2 mol L-1 in nitrate medium, with a practical detection limit of (4,98 ± 0,11)x10-4 mol L-1. For sulphate ions the PbO2 electrode did not responded directly. These ions might be dosed indirectly by potentimetric titration with standard Pb(II) solution in acidic media, in 1:1 ethanol-water (v/v), with good definition of the equivalence volumes. The reprodutibilidade of the potenciais and of the equivalence volumes obtained in samples with concentration at milimolar level in sulphate, indicate the possibility of the use of this electrode in quantifying sulphate ions.

As antocianinas, pigmentos da classe dos flavonóides, são os principais substâncias cromogênicas encontrados nas flores vermelhas, azuis e púrpuras. Uma das principais características das antocianinas, com aproveitamento didático é a sua mudança de coloração em função do pH do meio. Este trabalho se insere em um projeto mais amplo, que visa propor experimentos simples e de baixo custo para ensino, utilizando-se de vegetais facilmente encontrados no Brasil. Os corantes utilizados se prestam ao ensino desde conceitos básicos de equilíbrio químico para estudantes de ensino médio, de indicadores em titulação para cursos de química geral e até da Lei de Lambert-Beer e de Espectros de Absorção, para cursos de instrumentação. A espécie utilizada foi Solanum nigrum L (maria-preta), cujo extrato bruto foi utilizado como agente cromóforo. Usando o extrato bruto como indicador em titulações ácido-base, observaram-se erro relativos da ordem de 0,11-1,0%, quando comparado com os resultados potenciométricos. A mudança de cor observada foi de vermelho para amarelo, entre pH 4 e 10. Espectros de absorção na região do UV e do visível foram obtidos em diferentes pH, para determinação dos comprimentos de onda dos máximos de absorção, bem como para demonstração da mudança da forma destes espectros em função da acidez do meio.

Anthocyanins, pigments of flavonoids class, are the most important chromophors found in blue, red and purple vegetal tissues, whose color changes depending on the pH. The goal of this work was to propose a simple and cheap experiment to chemical education, using vegetal species easily found in Brazil. Such class of comounds presents a potential interest to students and teachers alike, to be useful in illustrating chemical principles such as acid-base equilibria, pKa, light absorption, effects of changes in conjugated double bounds, etc. The specie used was Solanum nigrum L (maria-preta) whose fruits crude extract was used to obtain molecular absorption spectra, to verify the Lambert-Beer law and as an indicator in acid-base titrations. The end point results obtained with the crude extracts when compared to the glass electrode ones showed relative errors between 0,1 and 1,0%. The color changed from red to yellow between pH 4 and 10. To determine the highest absorption wavelenght and demonstrate the shape changing of spectra in function of the acidity, the absorption spectra in UV and visible regions were obtained in different pH values.