Alteração do comportamento eletroquímico do eletrodo de níquel, em ácido sulfúrico diluído, sob diferentes condições de iluminação

In this paper is presented electrochemical evidences of the influence of the light on the electrochemical behavior of nickel electrode in diluted sulfuric acid. The current densities related with the electrooxidation of the metal decreases when the electrode is under illumination. The corrosion potential, Ecorr , shift to a more positive value in this condition. This effect was observed with polychromatic light and with different wavelength glass filters such as 700 nm and 520 nm. It was observed that increasing the temperature of the solution, the current densities related with cathodic and anodic processes, increases instead of decreases. The activation energy related with the electrooxidation of the electrode was higher under illumination than in the dark. It is suggested that this behavior may be related or with a photo-inhibition effect either with dessorption of adsorbed water involved in the electrooxidation mechanism.

Determinação de elementos-traço: relatório de dois exercícios interlaboratoriais

Results of two intercomparison exercises are reported. In the first one, the participants were asked to determine Cd, Cu, Pb and Zn, at the sub mg mL-1 level, in an acidified aqueous solution. In the second one, the participants were asked to determine mercury (total) in two homogeneous biological samples, hair and fish. The exercises were considered satisfactory and few reported results were discharged (3s criteria).

Eletrodos artesanais para voltametria

This paper describes the construction and performance of homemade electrodes for voltammetric purpose using cheap materials, like pipette tips and asbestos fiber. A good cost-to-benefit relation makes this devices specially designed for student use, expecting to improve the broadcasting of electroanalytical methods in Brazilian schools.

Redução seletiva aplicada à especiação de mercúrio em peixes: uma adaptação do método de Magos

In the selective reduction procedure proposed by Magos SnCl2 was used as reductant for inorganic mercury while total mercury was determined after reduction with a mixture of SnCl2 and CdCl2. The difference between total mercury and inorganic mercury determines the content of organic mercury. The procedure of the present work differs of Magos in that the mercury vapour is carried to the absorption cell after magnetic stirring of the solution in the reaction flask; in the Magos procedure, mercury vapour is carried by bubbling the gas in to the solution. In contrast to the Magos procedure this slight modification overcame the necessity of at calibration by analyte addition, saving time and gainning accuracy.

Sistema automático para determinação seqüencial de cianeto livre e total empregando eletrodo tubular íon-seletivo de membrana homogênea

This study presents an automated system for potentiometric determination of free and total cyanide which employs a homogeneous membrane tubular ion-selective electrode. After the electrode is assembled, it is connected to a system composed of 3 three-way solenoid valves, sample line, carrier line, acid stream, and gas diffusion chamber. A Turbo Pascal® computer program, developed specifically for this task, automatically performs all the steps involved in data acquisition and processing. The proposed analytical procedure offers operational simplicity, since detection is performed by a tubular electrode, whose assembly is fast and easy. The system has shown reproducibility (r.s.d. < 0.5%, n=6) and high speed (30 readings/hour); it is efficient for determination of free and total cyanide in waste waters of starch processing plants. The detection limit was 1.2x10-5 and 1.5x10-5 mol L-1, for determination of free and total cyanide, respectively. The linear response range was between 1.2x10-5 and 1.0x10-2 mol L-1 for free cyanide and between 1.5x10-5 and 1.0x10-2 for total cyanide.

Testes de desempenho de eletrodos: eletrodos de referência

This paper is designed to divulge some tests found in books, articles and international technical standards, by means of which it is possible to evaluate the performance of reference electrode widely used in potentiometric and voltammetric methods. The reference potential (Eref), junction resistance (Rj), the ability of keeping up the potential when current is flowing (polarizability), and of generating junction potentials (Ej) are applied to some commercial electrodes. The results obtained are amply discussed and some corrective procedures are suggested when the electrode fails.

Acoplamento cromatografia gasosa - espectrometria de absorção atômica em estudos de especiação: uma revisão

This review presents an updated overview of the trace element speciation by gas chromatography coupled with atomic absorption spectrometry.

Relato de uma experiência: recuperação e cadastramento de resíduos dos laboratórios de graduação do Instituto de Química da Universidade Federal do Rio Grande do Sul

An experience aiming to promote a residue interchange and recovery between the teaching laboratories of the Chemistry Institute of this University is described. At the present, several residues interchange have already appeared as advantageous. To make the work easier, a software has been developed in order to keep a record of all the residues generated by the teaching laboratories. Standard labels have been developed for the residues in order to organize them. The software and the label design are described.

A geração química de vapor em espectrometria atômica

The historical development of atomic spectrometry techniques based on chemical vapor generation by both batch and flow injection sampling formats is presented. Detection via atomic absorption spectrometry (AAS), microwave induced plasma optical emission spectrometry (MIP-OES), inductively coupled plasma optical emission spectrometry (ICP-OES) , inductively coupled plasma mass spectrometry (ICP-MS) and furnace atomic nonthermal excitation spectrometry (FANES) are considered. Hydride generation is separately considered in contrast to other methods of generation of volatile derivatives. Hg ¾ CVAAS (cold vapor atomic absorption spectrometry) is not considered here. The current state-of-the-art, including extension, advantages and limitations of this approach is discussed.

Quimiometria II: planilhas eletrônicas para cálculos de planejamentos experimentais, um tutorial

This work describes, through examples, a simple way to carry out experimental design calculations applying an spreadsheets. The aim of this tutorial is to introduce an alternative to sophisticated commercial programs that normally are too complex in data input and output. An overview of the principal methods is also briefly presented. The spreadsheets are suitable to handle different types of computations such as screening procedures applying factorial design and the optimization procedure based on response surface methodology. Furthermore, the spreadsheets are sufficiently versatile to be adapted to specific experimental designs.

Influência da espessura nas propriedades de absorção e emissão e na morfologia de filmes automontados de poli(p-fenileno vinileno)

In this report, we studied the thickness effect on the optical and morphological properties of self-assembled (SA) poly(p-phenylenevinylene) (PPV) films, wich were processed with 5 and 75 layers from a PPV precursor polymer and dodecylbenzenesulfonate, and then, thermally converted at 230 °C. The increase of the film thickness yielded more intense peaks in the vibrational spectral range. The electron-phonon coupling was quantified by the Huang - Rhys factor, that shows the effects on the polymer chain mobility in the interface substrate/polymer. A strong emission anisotropy r=0.57 was observed for the film with 5 layers of thickness decreasing to 0.34 for the film with 75 layers. Finally, the surface topology of the films was measured using Atomic Force Microscopy.

Mercury in soils and sediments from gold mining liabilities in Southern Amazonia

The 1980-1990 Amazonian gold rush left an enormous liability that increasingly has been substituted by developing fish aquaculture. This work aimed at the identification of the mercury levels in the environment, associated with fish farms located in the North of Mato Grosso State, Southern Amazon. Sediment and soil samples were analyzed for total organic carbon and total mercury. Results indicate that the chemical characteristics of the sediment largely depend on the management procedures of the fish pond (liming, fish food used and fish population). The soils presented relatively low concentrations when compared with other data from the literature.

Ondas ultrassônicas e pérolas de vidro: um novo método de extração de beta-galactosidase para uso em laboratório

The optimization of a traditional technique of cellular disruption by abrasion was carried out and a process using ultrasonic waves associated with glass pearls to extract beta-galactosidase from Kluyveromyces marxianus proposed. In the first case, the effects of the diameter and weight of the pearls in relation to the volume of cellular suspension and amount of time for cellular disruption were evaluated. The efficiency of the new process of cellular disruption was evaluated by varying the length of time of sonification and comparing with the method of abrasion under the same conditions. The proposed method can be efficiently applied to obtain beta-galactosidase at laboratory scale.

Desarrollo de un modelo SIMCA para la clasificación de kerosinas mediante el empleo de la espectroscopía infrarroja

In the petroleum refining industry, the use of crude from several origins is frequent. This leads to a product of variable chemical composition during refining, hindering quality control. Therefore, it is important to develop classification models that help to better characterize those products. The objective of this study is to develop a SIMCA recognition pattern to classify kerosene using infrared spectroscopy data. The model permits to differentiate two kerosene groups with different chemical compositions, which was corroborated by mass spectrometry.

Caracterização de escamas do peixe piau (Leporinus elongatus) e sua aplicação na remoção de Cu(II) de meio aquoso

Characterization of fish scales of Leporinus elongatus and their application in the removal of Cu(II) from aqueous solutions are described. It was observed that the scales are mainly formed by hydroxyapatite and type I collagen. Adsorption of Cu(II) was performed using batch experiments at 25 0C. The ANOVA statistical results have shown that the Langmuir model was successful applied to determine the maximum adsorption capacity of 2.686 x10-4 mol g-1 and the Langmuir equilibrium parameter (b) of 168.8 L mol-1. The Langmuir separation parameter, R L, has shown favorable adsorption of Cu(II) on the scales.