Efecto de la naturaleza del precursor sobre las caracteristicas de las nanoparticulas de SnO2 sintetizadas

Tin oxide (SnO2) is widely used in industry as raw material for electronic devices, plating of different types of materials, for dyes and pigments, for electroplating, heterogeneous catalysis, etc. In this work SnO2 was obtained by a controlled precipitation method with special attention to the effects the tin precursor has on the microstructure of the final product. The most appropriate pH for obtaining SnO2 with the rutile structure as the main phase is 6.25 for SnCl2 and 6.40 for SnSO4. After heat treatment at 600 °C, particles of nanometric order (~10 - 30 nm approx) were obtained. The characterization of the solid phase was made by X-ray diffraction (XRD), thermal analysis (DTA/TG), transmission electron microscopy (TEM) and Fourier transformed infrared spectroscopy (FTIR).

Determinação do coeficiente de atividade na diluição infinita (g¥) através da micro-extração em fase sólida (SPME)

In this study a new approach, solid phase micro extraction (SPME), is used in the evaluation of the infinite dilution activity coefficient of the solute in a given solvent. It is the purpose of the current work to demonstrate a different approach to obtain the data needed for studying the solution thermodynamics of binary liquid mixtures as well as for designing multi-component separations. The solutes investigated at the temperature 298.15 K were toluene, ethyl benzene and xylene in the solvent methanol.

Investigation of the occurrence of pesticide residues in rural wells and surface water following application to tobacco

In this work the exposure of wells and surface water to pesticides, commonly used for tobacco cropping, was assessed. Water consumption wells and surface water flows were sampled at different times. After a preconcentration step with solid phase extraction (SPE), the selected pesticides were determined by gas chromatography with electron capture detection (GC-ECD) or high performance liquid chromatography with diode array detection (HPLC-DAD). No pesticides were detected in the well water samples and surface water flow in the winter season. However, in the spring and summer higher concentrations of chlorpyrifos and imidacloprid were found in the water source samples. Atrazine, simazine and clomazone were also found. The occurrence of pesticides in collected water samples was related with the application to tobacco.

Un método de bajo costo para la determinación de cobre a nivel de vestigios en matrices de interés ambiental por espectrofotometría en fase sólida (EFS)

A method for determining copper by solid phase spectrophotometry (SPS) was optimized using the Doehlert design. Copper(II) was sorbed on a styrene-divinylbenzene anion-exchange resin as a Cu(II)-1-(2-pyridylazo)-2-naphthol (PAN) complex, at pH 7.0. Resin phase absorbances at 560 and 800 nm were measured directly. The detection limit was found to be 2.5 µg L-1. The relative standard deviation on ten replicate determinations of 10 µg Cu(II) in 1000 mL samples was 1.1%. The linear range of the determination was 5.0-100 µg L-1. The method was applied successfully to the determination of Cu(II) in natural water and vegetable samples.

Desenvolvimento e validação de método de análise de glifosato em grãos de soja

The main objective of this work is to develop an efficient procedure to determine glyphosate in soybean grains. The cleanup of the aqueous extracts was done in two steps, beginning with liquid-liquid partitioning and then solid-phase extraction with anion exchange resin. After derivatization with a mixture of trifluoroacetic anhydride (TFAA) and trifluoroethanol (TFE), quantification was done by gas chromatography coupled to mass spectrometry. The mean recovery and RSD of the spiked samples were, respectively, 80.5% and 3.1% at level 0.200 mg kg-1, 93.3% and 18.7% at level 0.500 mg kg-1 and 92% and 3.5% at level 1.000 mg kg-1. The method was linear in the working range (correlation coefficient = 0.9965).

Determinação de paládio em amostras biológicas aplicando técnicas analíticas nucleares

This study presents Pd determinations in bovine tissue samples containing palladium prepared in the laboratory, and CCQM-P63 automotive catalyst materials of the Proficiency Test, using instrumental thermal and epithermal neutron activation analysis and energy dispersive X-ray fluorescence techniques. Solvent extraction and solid phase extraction procedures were also applied to separate Pd from interfering elements before the irradiation in the nuclear reactor. The results obtained by different techniques were compared against each other to examine sensitivity, precision and accuracy.

Análise de resíduos de agrotóxicos em tomates empregando dispersão da matriz em fase sólida (DMFS) e cromatografia gasosa

This work was aimed on optimization of the matrix solid-phase dispersion (MSPD) technique using gas chromatography for analyzing residues of chlorpyriphos, λ-cyhalothrin, cypermethrin and deltamethrin in tomatoes. The results showed that silica was more efficient for the clean up of extracts, but florisil provided the highest recovery rates. A 2³ complete factorial design was carried out to evaluate the absorbent/sample ratio, presence of co-column (silica) and ultrasonic bath on the extraction rate. The percentage of extraction of the pesticides chlorpyriphos, λ-cyhalothrin, cypermethrin and deltamethrin were 64.7, 88.3, 99.2 and 89.2%, respectively, with relative standard deviations below 5%.

Rapid and accurate hplc-dad method for the determination of the herbicide bispyribac-sodium in surface water, and its validation

A new method is described for the determination of the herbicide bispyribac-sodium in surface water, especially from river and irrigated rice water samples. The method involves extraction in solid phase and quantification by high performance liquid chromatography with diode array detection (HPLC-DAD). After optimization of the extraction and separation parameters, the method was validated. The method presented average recoveries of 101.3 and 97.7%, under repeatability and intermediate precision conditions, respectively, with adequate precision (RSD from 0.9 to 7.5%). The method was applied for the determination of bispyribac-sodium in surface water samples with a limit of detection of 0.1 μg L-1.

QuEChERS: um método moderno de preparo de amostra para determinação multirresíduo de pesticidas em alimentos por métodos cromatográficos acoplados à espectrometria de massas

This review attempts to provide an updated overview of the Quick, Easy, Cheap, Effective, Ruged and Safe (QuEChERS) multiresidue extraction method, that involves initial extraction in acetonitrile, an extraction/partition step after the addition of salt, and a cleanup step utilizing dispersive solid phase extraction. QuEChERS method is nowadays the most applied extraction method for the determination of pesticide residues in food samples, providing acceptable recoveries for acidic, neutral and basic pesticides. Several applications for various food matrices (fruits, vegetables, cereals and others) in combination with chromatographic mass spectrometry analysis were presented.

Determinação de resíduos de pesticidas em plasma bovino por cromatografia gasosa-espectrometria de massas

An analytical method for the isolation based on matrix solid-phase dispersion technique and gas chromatographic determination of pesticides in cattle plasma is presented. It was fortified 0.25 g of plasma with pesticides and blended with 1 g each C18 and Na2SO4. The homogenized matter was transferred to a SPE cartridge, which contained 1 g of activated florisil with 5 mL acetonitrile. The analites were eluted under vaccum with 15 mL acetonitrile, the extract was analyzed by gas chromatography-mass spectrometry. The limit of quantification of the method was 0.04 mg L-1 for chlorphenvinfos and fipronil and 0.02 mg L-1 for cypermethrin..

Estudo da sorção do corante catiônico violeta cristal por espuma de poliuretano em meio aquoso contendo dodecilsulfato de sódio

This work presents a detailed study about the sorption of crystal violet (CV) cationic dye onto polyether type polyurethane foam (PUF). The sorption process was based on the formation of an ionic-pair between cationic dye and dodecylsulfate anion (SDS), which presented high affinity by PUF. Set-up employed in the study was built up by adjusting a 200 mg cylinder of PUF to the arm of an overhead stirrer. The system was characterized in relation to equilibrium and kinetic aspects and it was modeled by employing Langmuir and Freundlich isotherms. Obtained results showed that the ratio between SDS and MB concentrations played an important role on the sorption process. According to results found it was possible to retain up to 3.4 mg of dye from 200 mL of a 5.0 x 10-5 mol L-1 CV solution containing 1.25 x 10-4 mol L-1 SDS, which represented a removal efficiency of around 92%.

Enriquecimento de compostos fenólicos de folhas de Inga edulis por extração em fase sólida: quantificação de seus compostos majoritários e avaliação da capacidade antioxidante

A phenolic fraction was obtained from of the acetone-water-acetic acid extract of Inga edulis leaves, by liquid-liquid partition and SPE-C18 cartridges. This method provided an increase of 108, 66, 51, 50 and 36% of flavonols, proanthocyanidins, total polyphenols, gallotannins and flavanols, respectively. The major phenolics in purified fraction were procyanidin B2, catechin and myricetin-3-O-α-L-rhamnopyranoside, which achieved increases of 111, 47 and 45%, respectively, after SPE. Acid hydrolysis confirmed the presence of procyanidins, prodelphinidins and glycosylated flavonoids.

Sistema limpo em linha para extração em fase sólida de contaminantes emergentes em águas naturais

A solid-phase in-line extraction system for water samples containing low levels of emerging contaminants is described. The system was specially developed for large volume samples (up to 4 L) using commercial solid-phase extraction (SPE) cartridges. Four sets containing PTFE-made connectors, brass adapters and ball valves were used to fit SPE cartridges and sample bottles to a 4-port manifold attached to a 20 L carboy. A lab-made vacuum device was connected to the manifold cap. The apparatus is robust and less expensive than the typical available system. Its also provides less experimental handling, avoiding cross contamination and sample losses.

Caracterização de contaminantes presentes em sistemas de tratamento de esgotos, por cromatografia líquida acoplada à espectrometria de massas tandem em alta resolução

This work shows results on the characterization, by liquid chromatography coupled to high resolution tandem mass spectrometry (LC-IT-TOF-MS) with electrospray ionization, of organic compounds present in raw and treated effluents from a combined sewage treatment systems (upflow anaerobic sludge blanket-trickling filter). The sewage samples were prepared by C18 solid phase extraction and the spectra obtained from the various extracts were submitted to principal component analysis to evaluate their pattern and identify the major deprotonated species. Some target compounds were submitted to semiquantitative analysis, using phenolphtalein as internal standard. The results showed the anaerobic step had little impact on the removal of anionic surfactants (LAS), fatty acids, and some contaminantes such as bisphenol A and bezafibrate, whereas the aerobic post-treatment was very efficient in removing these organics.

Síntese, caracterização e estudos de interação de um análogo da antitoxina CcdA empregando fluorescência no estado estacionário

Toxin-antitoxin (TA) systems contribute to plasmid stability by a mechanism called post-segregational killing. The ccd was the first TA system to be discovered with CcdB being the toxin and CcdA the antitoxin. CcdA, an 8.3 kDa protein, interacts with CcdB (11.7 kDa), preventing the cytotoxic activity of CcdB on the DNA gyrase. As an approach to understanding this interaction, CcdA41, a polypeptide derived from CcdA, was synthesized by solid-phase methodology and its interaction with CcdB was analyzed by steady state fluorescence. CcdA41 formed a stable complex with CcdBET2, a peptide based on CcdB, the more recently described bacterial topoisomerase inhibitor.