Método colorimétrico para determinação de dióxido de nitrogênio atmosférico com preconcentração em coluna de c-18

An alternative analytical method for nitrogen dioxide (NO2) in atmosphere was developed. The collection of NO2 is performed by a Sep-Pack C-18 cartridge impregnated with 11% (v/v) of triethanolamine plus 3,6 % (v/v) of ethylene glycol plus 25 % (v/v) of acetone combined solution. When the impregnating is used, NO2 is collected with good repeatibility (CV = 3,3 %). The NO2 absorbed in the sampler was stripped from the sorbent with a methanol 5% (v/v) aqueous solution and was determined by colorimetry as nitrite by using the Griess-Saltzman reagent. The detection limit of 1,4 ppb for 60 min sampling at 0,5 L min-1 flow rate was obtained. Preparation and conditioning procedures for TEA-C-18 cartridge, sampling flow rate, absorption capacity and interference of other species are discussed.

Utilização de índices r e R obtidos de programas interlaboratoriais para o controle de precisão de método analítico: Determinação de água por Karl Fischer

Values of repeatability (r) and reproducibility (R) are parameters of an analytical method. They are related to the maximum difference between two results of analysis (permissible range) and can be obtained by interlaboratorial comparisons. They represent great importance for the quality control of the results and decisions about the fitness-for-purpose of the method. Water determination in fuel oil samples were performed by 16 laboratories, using the Karl Fischer reaction, during the period from June 1997 to December 1999. Values of r and R were presented. Discussion is made in terms of the main factors that would be contribution to analytical method variabilities and uncertainties of final results.

Síntese de membranas cerâmicas via método sol-gel utilizando TEOS e N,N-dimetilformamida

In this work we obtained microporous and mesoporous silica membranes by sol-gel processing. Tetraethylortosilicate (TEOS) was used as precursor. Nitric acid was used as catalyst. In order to study the affect of N,N-dimethylformamide (NDF) as drying additive, we used a molar ratio TEOS/NDF of 1/3. The performance of N,N-dimethylformamide was evaluated through monolithicity measurements. The structural evolutions occurring during the sol-gel transition and in the interconnected network of the membranes during thermal treatment were monitored by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analyses and nitrogen sorption. We noted that in the presence of N,N-dimethylformamide, polymerization goes through a temporary stabilization of oligomers. The Si-O(H) bonds are stronger and belong to a more cross-linked structure for the N,N-dimethylformamide containing sol. The membranes obtained in the presence of N,N-dimethylformamide have larger surface area and its pore structure is in the range of mesoporous. The membranes obtained without additive have pore structure in the range of microporous.

Preparação de LiNbO3 e LiNbO3:Eu3+ pelo método dos precursores poliméricos

The ferroelectric compound LiNbO3 was prepared by the polymeric precursors method in the polycrystalline form containing different concentrations of Eu3+. The compounds were characterized by X-ray diffraction, vibrational and electronic spectroscopy. Electronic spectroscopy was shown to be sensitive to small concentrations of contaminating phases allowing a good control of the compound purity. The presence of Eu3+ ions leads to the formation of the LiNb3O8 phase in the range of 500 to 800 °C. Above this temperature range LiNbO3 and tetragonal (T') EuNbO4 were obtained.

Determinação de As em amostras orgânicas de interesse ambiental por espectrometria de absorção atômica com atomização eletrotérmica após combustão em bomba de O2

The toxicity of the major As species present in the environment justifies the effort for quantifying the element in environmental organic samples, which can vary from animal and vegetal tissues to coal and industrial residues. This paper comments about the applicability of the O2 bomb digestion, as a general procedure for all environmental organic materials. A rapid and straightforward method is suggested, which consists in burning the sample in the bomb at high O2 pressure, dissolving the vapours in diluted HNO3 and determining As in the resulting solution by atomic absorption spectrometry with electrothermal atomization. The method was applied to certified materials and plant samples.

Construção de uma fonte de corrente e de uma sonda para medida de condutividade pelo método da sonda de quatro pontas

This paper describes the construction of an eletrical current source and of a probe to be used in the measurement of eletrical conductivity through a four-point probe method. These pieces of equipments can be obtained at the low price of US$ 50.00 and are adequate for eletrical conductivity measurements in the semiconductor range, that is from 10-1 to 10-6 S cm-1.

Determinação de tanino em pedúnculo de caju: método da vanilina versus método do butanol ácido

To improve tannin assay in cashew apple, several parameters were examined, including (1) extraction solvents, (2) effects of water and boiling time on butanol acid reaction and (3) correlation between vanillin and butanol acid assay of tannin in cashew apples. The 50-70% acetone extracted the greatest amount of tannin from cashew apples. Concentrations of water in butanol reagents were adjusted and boiling time of butanol reaction was reduced at 15 min. Tannin of unripe cashew apples was purified on Sephadex LH-20, aiming to obtain tannin standard for butanol assay. The vanillin assay presented high correlation with the butanol acid assay.

O método das trajectórias clássicas: colisões coplanares do tipo A+BC

The general methodology of classical trajectories as applied to elementary chemical reactions of the A+BC type is presented. The goal is to elucidate students about the main theoretical features and potentialities in applying this versatile method to calculate the dynamical properties of reactive systems. Only the methodology for two-dimensional (2D) case is described, from which the general theory for 3D follows straightforwardly. The adopted point of view is, as much as possible, that of allowing a direct translation of the concepts into a working program. An application to the reaction O(¹D)+H2->O+OH with relevance in atmospheric chemistry is also presented. The FORTRAN codes used are available through the web page www.qqesc.qui.uc.pt.

Hidrogenação de compostos orgânicos utilizando método eletroquímico para geração de hidrogênio in situ: hidrogenação eletrocatalítica

Electrocatalytic hydrogenation (HEC) may be compared to catalytic hydrogenation (HC). The difference between these methods is the hydrogen source: HC needs a hydrogen gas supply; HEC needs a source of protons (solvent) to be reduced at a cathode surface. HEC has presented interesting advances in the last decades due to investigation of the influence of the supporting electrolyte, co-solvent, surfactant, presence of inert gas and the composition of the electrode on the reaction. Several classes of organic compounds have been hydrogenated through HEC: olefins, ketones, aldehydes, aromatics, polyaromatics and nitro-compounds. This paper shows some details about the HEC which may be regarded as a promising technique for the hydrogenation of organic compounds both in industrial processes and in laboratories.

A poluição gerada por máquinas de combustão interna movidas à diesel - a questão dos particulados. Estratégias atuais para a redução e controle das emissões e tendências futuras

The exhaust emissions of vehicles greatly contribute to environmental pollution. Diesel engines are extremely fuel-efficient. However, the exhaust compounds emitted by diesel engines are both a health hazard and a nuisance to the public. This paper gives an overview of the emission control of particulates from diesel exhaust compounds. The worldwide emission standards are summarized. Possible devices for reducing diesel pollutants are discussed. It is clear that after-treatment devices are necessary. Catalytic converters that collect particulates from diesel exhaust and promote the catalytic burn-off are examined. Finally, recent trends in diesel particulate emission control by novel catalysts are presented.

Adaptação no método do peso da gota para determinação da tensão superficial: um método simplificado para a quantificação da CMC de surfactantes no ensino da química

The discussion based on surfactant cleaning action is commonly used in chemistry classrooms for the comprehension of theoretical concepts related to surface tension and micelle formation. The experimental quantification of surface tension of aqueous solutions of surfactants provides the practical instruments for this discussion. The present paper describes a simplification on the common apparatus employed for the drop-weight method, making the determination of surface tension accessible to any chemistry lab. The surface tension of various liquids and the critical micelle concentration, CMC, of three commercial surfactants were measured with this modified method, and proved to be consistent with literature values.

Método de estudo da adsorção de triadimenol com micro-colunas de solo e centrifugação

Normally, the determination of equilibrium constants (k d) in batch experiments uses a high solution to soil ratio, which does not represent field conditions. In this study we present an alternative method to evaluate adsorption constants, using micro-columns of soil at higher soil to solution ratios. The centrifugation force and equilibration time were investigated. The triadimenol distribution along the column profile is controlled by diffusion and equilibration times greater than 24 h are needed to achieve reproducibility. The centrifugation force must be superior to 670 g in order to guarantee enough extraction of the liquid solution from the soil columns.

Validação do método de determinação simultânea dos íons brometo e bromato por cromatografia iônica em águas de consumo humano

European Directive (98/83/CE), compulsory after 2008, states that bromate in drinking water must be controlled at levels below 10 mg L-1. Supporting implementation of the Directive, the European Comission has established project SMT4-CT96 2134, in collaboration with various european institutions, aiming at the identification of the interferents to the current analytical method (Ionic Chromatography with Conductimetric Detection - IC/CD), their removal and the automation of pre-treatment and injection steps, as well as the development of alternative methods. EPAL, responsible for the water supply to a great deal of Portuguese regions, has taken steps to meet these requirements. Although not part of such project, this work (the result of a project conducted under a protocol of collaboration between EPAL SA and FCUL - Faculty of Sciences, University of Lisbon), reports on studies of usefulness to laboratories planning to monitor bromate in ozone treated waters, in conditions different from those described in EPA 300.1. Simultaneous determination of bromide is justified by its role as bromate precursor.

Hidrogenação eletrocatalítica de substratos orgânicos: estudo da eficiência dos metais nobres níquel, paládio e platina usando eletrodos modificados

Nickel, palladium and platinum micro-crystals were dispersed in films covering a vitreous carbon plate electrode by ion exchange followed by electroreduction of their ions. These modified electrodes were used in the electrocatalytic hydrogenation of several substrates of different classes and their efficiency is reported. A comparison among them was performed based on the structural characteristics of the metals. A modified electrode containing platinum showed to be more efficient than a palladium modified electrode and the one of nickel was the less efficient.

La radicalización Heideggeriana del método fenomenológico

Este trabajo quiere esclarecer cómo y por qué, en la doctrina del «primer» Heidegger,la hermenéutica emerge como el complemento metodológico indispensable para el transcendentalismo de la fenomenología. Constata que la afinidad metodológica es el vínculo decisivo entre esta doctrina y la ontología fundamental, en contraste con una manifiesta disparidad temática: la conciencia, la intencionalidad y la reflexión son tres cruciales referenciasfenomenológicas que carecen de contrapartida fundamental-ontológica. Pero si Heidegger preserva la dimensión transcendental recogida de la fenomenología, tambiénimprime a su doctrina un carácter específicamente hermenéutico, patente en la transformación que recibe la noción capital de Auslegung. Hermenéutica y transcendentalismo, en efecto,no sólo no son antagónicos sino que estjn armonizados en el rnodus operandi de la ontología fundamental. En su indagación del a priori de toda constitución de sentido, tributaria de un antideductivismo tan exacerbado como el de la fenomenología, Heidegger introduce una dimensión metodológica inédita. Al fin y al cabo, la automostración del ser no ocupa el lugar teórico, supuestamente ametódico, que la fenomenología asigna a la in-mediatez.Entender esta mutación del método fenomenológico, desde luego, conlleva explorar en detalle cómo integró Heidegger las dispares componentes doctrinales de la ontología fundamental y por qué se empeñó en cuestionar el carácter neutral que se suele exigir al método.Transponiendo el transcendentalismo presencialista de Husserl en un proyecto ontológico, reinterpretó la metodología de la «intuitividad presentificadora» hasta hacerla compatible con una noción radicalmente ampliada de fenómeno. Así una indagación fenomenológica legítima ha de investigar transcendentalmente el «sentido del ser» como el apriori absoluto.La fenomenología ha de ser realizada como ontología.