Mecanismos de Separação em Eletroforese Capilar

Since its inception in the 80's, capillary electrophoresis has matured into a well established technique for the separation and analysis of complex samples. One of its strongest aspects is the ability to handle materials from a diversity of chemical classes, ranging from few to millions of Daltons. This is only possible because several modes of electrophoresis can be performed in a single capillary format. In this work, relevant aspects of capillary zone electrophoresis in its three modes (free solution, micellar and gel), capillary isoelectric focusing and capillary isotachophoresis are discussed and many representative applications are presented.

Pervaporação: uma técnica de separação contínua não-cromatográfica

A brief discussion of the non-chromatographic continuous separation techniques is presented emphasizing the pervaporation process. It makes interesting choices for implementing various preliminary operations of the analytical process in order to accommodate the raw sample to the measuring instrument. Discussions include the perceived advantages and disadvantages, the underlying principles of pervaporation process, the flexible module and fields of application.

Determinação de potássio em méis após precipitação com tetrafenilborato de sódio e separação em coluna de troca-iônica

A new method for determination of potassium in honey samples of different colors was developed as an alternative method for determination of this metal. Analysis of genuine honeys attested by the qualities and quantities tests officially adopted in Brazil, showed that the concentration of potassium ranged from 181 to 315 mg/kg for light honeys, from 393 to 570 mg/kg for medium honeys and from 791 to 915 mg/kg for dark honeys. Recoveries making use of spikes of potassium added to the honey samples and to the deionized distilled water showed results close by hundred percent at pH <= 2,0 under temperature bellow 20°C.

Separação de espectros simulados e de luminescência total através do método generalizado de anulação do posto (GRAM)

A multivariate curve resolution method, "GENERALIZED RANK ANNIHILATION METHOD (GRAM)", is discussed and tested with simulated and experimental data. The analysis of simulated data provides general guidelines concerning the condition for uniqueness of a solution for a given problem. The second-order emission-excitation spectra of human and animal dental calculus deposits were used as an experimental data to estimate the performance of the above method. Three porphyrinic spectral profiles, for both human and cat, were obtained by the use of GRAM.

Determinação de Cd, Ni e Zn por espectrometria de emissão atômica com plasma indutivamente acoplado, após separação e pré-concentração em coluna contendo p-dimetilaminobenzilidenorodanina adsorvida sobre sílica gel

A column packed with 5-(4-dimethylaminobenzylidene)rhodanine adsorbed on silica gel was used for the preconcentration of Cd, Ni and Zn at different spiked solutions prior to their determination by inductively coupled plasma atomic emission spectrometry. This column allowed recoveries over than 98% for the above elements and accurate analyses of coastal sea-water certified reference material were also achieved.

Separação e identificação de constituintes químicos polares dos galhos de Porcelia Macrocarpa

This paper describes a methodology to separate and identify polar compounds as flavonoid and lignan glucosides, amino acids, salt of quaternary ammonium amino acid and carbohydrates from branches of Porcelia macrocarpa (Annonaceae).

Técnica para seleção de variáveis aplicada à separação de gases

This paper describes an experimental design technique, known as variables search, developed to expose the critical variables and screen out the irrelevant ones. It is easy to learn and use and clearly dissociates the main and interactions effects from each other. An example of air separation process by pressure swing adsorption was used to demonstrate how the variables search technique works. The phases of identification of the critical variables is shown, step by step,.

Experimentos didáticos em química analítica envolvendo separação de fases e pré-concentração

The aim of this work was to propose two different didactic experiments, which can be used in practical classes of analytical chemistry courses. More flexible experiments related to the theme, giving some options to the instructor are proposed. In this way, the Experiment 1 was divided in two parts. In the first one, the visualization of two distinct phases separation is emphasized: the rich and the poor phases in surfactant. In the second part, the metal pre-concentration (Co as example) is emphasized. The Experiment 2 has three different parts. In the first one, the complex formation is pointed out, in the second one, the pH influence is shown and in the last one, the influence of the complexation time is demonstrated.

Determinação de Mn, Cu e Zn em matrizes salinas após separação e pré-concentração usando Amberlite XAD-7 impregnada com Vermelho de Alizarina S

The aim of this work was to explore the possibility of the application of a non-ionic resin obtained by impregnation of Alizarin Red S (VAS) in Amberlite XAD-7 for manganese, copper and zinc separation and preconcentration in saline matrices. For these system, the metals were quantitatively retained, in the pH range 8.5-10.0, by using 0.50 g of solid phase, stirring time of five minutes and a total mass up to 200 mug of each cation. The sorbed elements were subsequently eluted and a fifty-fold, ten-fold and ten-fold preconcentration factor for to Zn, Cu and Mn were obtained, respectively.

Resinas poliméricas para separação e pré-concentração de chumbo

This article gives an overview of polymer materials used for lead separation and preconcentration. Different kinds of polymer resins, commercial or not, are cited as well as the most used functional groups attached to polymer backbones. The synthesis of these resins and conditions of lead adsorption and elution are remarked. The influence of the porous structure of the polymer on the resines performance is described as well as the use of spacer arms.

Separação de CO2 por meio da tecnologia PSA

This paper describes the separation of CO2 from a gas mixture containing 25% CO2, 4% O2 and 71% N2 using the pressure swing adsorption (PSA) technique. The adsorbent selected was the zeolite 13X due to its great adsorption capacity for CO2 and selectivity towards the other components of the gas mixture. The experimental technique was designed to identify the most important variables for the process and to optimize it. It is shown that the PSA technique can be used to separate CO2 from O2 and N2 to obtain an effluent containing 2% CO2 with 99% separation efficiency.

Polímeros biomiméticos em química analítica. Parte 1: preparo e aplicações de MIP ("Molecularly Imprinted Polymers") em técnicas de extração e separação

MIPs are synthetic polymers that are used as biomimetic materials simulating the mechanism verified in natural entities such as antibodies and enzymes. Although MIPs have been successfully used as an outstanding tool for enhancing the selectivity or different analytical approaches, such as separation science and electrochemical and optical sensors, several parameters must be optimized during their synthesis. Therefore, the state-of-the-art of MIP production as well as the different polymerization methods are discussed. The potential selectivity of MIPs in the extraction and separation techniques focusing mainly on environmental, clinical and pharmaceutical samples as applications for analytical purposes is presented.

Separação cromatográfica quiral de anestésicos a partir de soluções diluídas e concentradas em escala preparativa

In this work the separation of the chiral anesthetic compounds ketamine and bupivacaine was development using two chiral stationary phases (CSP). Ketamine enantiomers were well separate in the polysaccharide-based CSP (microcrystalline cellulose triacetate - MCTA) while bupivacaine in the tartardiamide-based CSP (Kromasil CHI-TBB). In both cases, the effect of temperature was investigated under analytical conditions. An improvement in the separation performance with temperature was observed. Thermodynamic parameters were evaluated by the van't Hoff plot. We concluded that enthalpic effects controlled the retention in these chiral columns. The enantiomers of ketamine and bupivacaine were separated under overloaded conditions with a good performance.

Estudo por espectroscopia micro-Raman dos mecanismos de separação de fase em vidros fosfatos de metais de transição

Glass-ceramics are prepared by controlled separation of crystal phases in glasses, leading to uniform and dense grain structures. On the other hand, chemical leaching of soluble crystal phases yields porous glass-ceramics with important applications. Here, glass/ceramic interfaces of niobo-, vanado- and titano-phosphate glasses were studied by micro-Raman spectroscopy, whose spatial resolution revealed the multiphase structures. Phase-separation mechanisms were also determined by this technique, revealing that interface composition remained unchanged as the crystallization front advanced for niobo- and vanadophosphate glasses (interface-controlled crystallization). For titanophosphate glasses, phase composition changed continuously with time up to the equilibrium composition, indicating a spinodal-type phase separation.

Separação semipreparativa de α e β-amirina por cromatografia líquida de alta eficiência

The resin obtained from species of the genus Protium (Burseraceae) is formed mostly of pentacyclic triterpenes: α-amyrin and β-amyrin. The separation and purification of these triterpenes were optimized in three steps.