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.

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.

Influência do agente precipitante na preparação do óxido de nióbio (V) hidratado pelo método da precipitação em solução homogênea

This work reports the preparation, characterization and study of the ion exchange behavior of hydrous niobium oxide prepared by a homogeneous precipitation method. The precipitating agent was obtained in aqueous solution by thermal decomposition of urea or ammonium carbonate. The compounds were chemically and physically characterized by X-ray diffractometry, thermal analysis (TG/DTG), surface area measurements and ion exchange behavior with sodium. The materials prepared with ammonium carbonate presented a higher degree of crystallinity and better ion exchange capacity with sodium than materials prepared with urea. In the homogeneous precipitation method, materials were obtained with specific surface area of 123 - 224 m² g-1. A variation of the preparation process produced hydrous niobium oxide with a different degree of hydration and specific surface area. This provided materials with different physico-chemical properties.

Método para a determinação de hexazinone e tebutiuron em água

This work presents an alternative method for determination of the herbicides tebuthiuron and hexazinone in ground water. The extraction was made with dichloromethane and the analyses by high performance liquid chromatography (HPLC), using reversed-phase column, C-18, mobile phase methanol/water 50:50, v/v, detection and quantification at 247 nm. The following validation parameters were obtained: limit of detection of method 0.02 and 0.03 µg L-1, limit of quantification of method 0.07 and 0.09 µg L-1; linear range limit of quantification of instrument - 300 µg L-1 (r² > 0.998); recoveries from 90.3 to 108.2% and 90.3 to 101.6%; intermediary precision (%RSD) < 8 and < 6%, for hexazinone and tebuthiuron, respectively. The method showed to be efficient and reliable for determination of the herbicides in ground water.

Síntese de indanos: uma seleção de métodos gerais e eficientes

The indan ring system is present in several compounds with important pharmacological properties. In this account recent examples of selected methods (Friedel-Crafts acylation, cycloaddition reactions, ring contraction, cyclization and resolution) for the synthesis of indans are discussed.

Caracterização de cimento odontológico obtido a partir de um vidro preparado pelo método dos precursores poliméricos

Glass ionomer cements are glass and polymer composite materials. These materials currently find use in dentistry. The purpose of this work is to obtain glass powders based on the composition 4.5SiO2 - 3Al2O3 - 2CaO to be used in dentistry. The powders were prepared by a chemical route at 700 0C. The properties of glass ionomer cements obtained from powders prepared at 700 ºC were studied. Diametral tensile strength and microhardness were evaluated for the experimental glass ionomer cements and a commercial material. It was concluded that the properties of experimental cements were similar to those of the commercial ones.

Determinação das formas de nitrogênio e nitrogênio total em rochas-reservatório de petróleo por destilação com arraste de vapor e método do indofenol

Several extraction procedures are described for the determination of exchangeable and fixed ammonium, nitrate + nitrite, total exchangeable nitrogen and total nitrogen in certified reference soils and petroleum reservoir rock samples by steam distillation and indophenol method. After improvement of the original distillation system, an increase in worker safety, a reduction in time consumption, a decrease of 73% in blank value and an analysis without ammonia loss, which could possibly occur, were achieved. The precision (RSD < 8%, n = 3) and the detection limit (9 mg kg-1 NH4+-N) are better than those of published procedures.

Cálculos teóricos de afinidades por próton de n-alquilaminas usando o método ONIOM

The ONIOM method was used to calculate the proton affinities (PA) of n-alkylamines (CnH2n+1NH2, n = 3 to 6, 8, 10, 12, 14, 16 and 18). The calculations were carried out at several levels (HF, MP2, B3LYP, QCISD(T), ...) using Pople basis sets and at the QCISD(T) level using basis sets developed by the generator coordinate method (GCM) and adapted to effective core potentials. PAs were also obtained through the GCM and high level methods, like ONIOM[QCISD(T)/6-31+G(2df,p):MP2/6-31G+G(d,p))//ONIOM[MP2/6-31+G(d,p):HF/6-31G]. The average error using the GCM, with respect to experimental data, was 3.4 kJ mol-1.

Análise quiral por espectrometria de massas através da utilização do método cinético

Novel and quantitative mass spectrometry methods for rapid and accurate enantiomeric excess determination are presented. These methodologies use electrospray ionization (ESI) and mass spectrometry (MS) to detect and analyze, via collision-induced dissociation (CID), mass-selected transition metal complexes that promote enantio especific interactions. The data from CID are conveniently treated by the kinetic method, a sensitive linear free energy method of treating mass spectrometric results. Four different variations of this methodology are described: single ratio method (S R), quotient ratio method (Q R), fixed ligand method (S Rfixed), and quotient ratio method with fixed ligand (Q Rfixed). These individual methods are compared and their main features discussed in detail.

Incorporação de CuSO4 residual em argamassa, como método de disposição final

Residual CuSO4 was incorporated into the mass utilized for cement preparation. To a cement mass with 1:0.5:5 of cement, lime and sand to 0.25, 0.50, 0.75 and 1.00% of residual CuSO4 were added. The sulfate was mixed separately with lime and water to induce metal precipitation. The hardened test bodies were submerged in Milli-Q water for three months. No Cu was detected in the water by Atomic Absorption Spectrometry. The best proportion for mechanical resistance and porosity is 0.50%. The cement is adequate for non-structural objects.