Otimização e validação da extração sólido-líquido e purificação em baixa temperatura de HPAs em lodo de esgoto

In this study, a method of solid-liquid extraction and purification at low temperature (SLE-PLT) to determine 16 polycyclic aromatic hydrocarbons (PAHs) in sewage sludge was optimized and validated. The analyses were performed by HPLC-UV. The extraction phase, homogenization procedure, influence of pH, ionic strength and clean-up of the extracts were optimized. Recoveries were higher than 63.4% for 11 PAHs. The correlation coefficients were greater than 0.99 and limits of detection and quantitation were less than 0.060 and 0.15 µg g-1, respectively. These values were lower than the maximum residue limits of PAHs established by European legislation. SLE-PLT proved a more practical, economical method with fewer steps compared to Soxhlet extraction (reference method) for PAHs in sewage sludge.

Remoção de compostos fenólicos de soluções aquosas utilizando carvão ativado preparado a partir do aguapé (Eichhornia crassipes): estudo cinético e de equilíbrio termodinâmico

Activated carbon was produced from the water hyacinth (CAA) by impregnation with ZnCl2 (1:2), followed by pyrolysis at 700 ºC, under N2. CAA was used for the adsorption of phenol, m-cresol and o-cresol from aqueous solutions, using batch adsorption. The effects of contact time, pH, temperature and concentration on sorption were investigated. Adsorption capacity, calculated using the Langmuir model proved to be dependent on temperature, reaching values of 163.7, 130.2 and 142.3 mg g-1 for phenol, m-cresol and o-cresol, respectively, at 45 ºC. Thermodynamic data at the solid-liquid interface suggests an endothermic, spontaneous and environmentally-friendly process.

Adsorção de alfa-lactalbumina do soro de leite em hidroxiapatita: efeito do pH e da temperatura e análise termodinâmica

The nutritional and functional benefits offered by whey protein α-lactalbumin justify the great interest in its manufacture in large quantities at a high purity level. Hydroxyapatite is a calcium phosphate material able to adsorb proteins and can be synthesized at low production cost. Therefore, this work evaluated the adsorption of α-lactalbumin on hydroxyapatite using solid-liquid phase equilibrium data reported as adsorption isotherms. Van't Hoff's thermodynamics analysis showed that the adsorption process is entropically driven.

APARATO ELETROQUÍMICO PARA SISTEMA DE AQUISIÇÃO DE DADOS MULTICANAL COM RESOLUÇÃO ESPAÇO-TEMPORAL

Spatiotemporal pattern formation in reaction-transport systems takes place spontaneously when the system is kept far from thermodynamic equilibrium. Targets, reaction fronts, waves, spirals, spots and stripes are some typical examples of selforganized structuring. In electrochemical systems, monitoring spatiotemporal patterns of potential in the solid/liquid interface can be done by the use of equally distributed microprobes located close to the working electrode. However, the physical size of each probe can limit the spatial resolution and alter mass transport properties. In contrast, the direct measurement of discrete electrodes does not suffer from this limitation and allows the accurate manipulation of the spatial coupling through changes in resistors connected to the electric circuit. In this paper, the development of an electrochemical setup for multichannel data acquisition with spatiotemporal resolution is described, especially to monitor low levels of currents usually observed in the electro-oxidation of small organic molecules.

PREPARO DE AMOSTRAS ASSISTIDO POR CAMPO ELÉTRICO: FUNDAMENTOS, AVANÇOS, APLICAÇÕES E TENDÊNCIAS

Sample preparation is commonly considered a key step to achieve selective, sensitive, and reliable chemical analyses, particularly those involving complex matrices. Although the application of electric fields to improve the speed and efficiency of sample preparation methods has been proven, this approach is still considered to be state-of-the-art; hence, further development is necessary to improve future applications. This review describes the fundamentals, advances, applications, and perspectives of using electric fields to enhance sample preparation techniques such as liquid-liquid and solid-liquid extractions in conventional and microscale devices.

Determination of fipronil in bovine plasma by solid-phase extraction and liquid chromatography with ultraviolet detection

A fast and efficient method has been developed and validated for the determination of fipronil in bovine plasma. Samples were subjected to solid-phase extraction (SPE) followed by reversed phase liquid chromatography (LC) separation, using acetonitrile/water (60:40 v/v) as the mobile phase with a flow rate of 1.0 mL/min and ultraviolet (UV) detection at 210 nm. Ethiprole was used as the internal standard (IS). The method was found to be linear over the range 5-500 ng/mL (r = 0.999). The limit of quantitation (LOQ) was validated at 5 ng/mL. The method was successfully applied to monitor plasma concentrations following subcutaneous administration of fipronil in cattle.

Dispersive liquid-liquid microextraction for the simultaneous separation of trace amounts of zinc and cadmium ions in water samples prior to flame atomic absorption spectrometry determination

In the proposed method, carbon tetrachloride and ethanol were used as extraction and dispersive solvents. Several factors that may be affected on the extraction process, such as extraction solvent, disperser solvent, the volume of extraction and disperser solvent, pH of the aqueous solution and extraction time were optimized. Under the optimal conditions, linearity was maintained between 1.0 ng mL-1 to 1.5 mg mL-1 for zinc and 1.0 ng mL-1 to 0.4 mg mL-1 for cadmium. The proposed method has been applied for determination of trace amount of zinc and cadmium in standard and water samples with satisfactory results.

Dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous separation/preconcentration of nickel, cobalt and copper prior to determination by electrothermal atomic absorption spectrometry

A dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous extraction of trace amounts of nickel, cobalt and copper followed by their determination with electrothermal atomic absorption spectrometry was developed. 300 µL of acetone and 1-undecanol was injected into an aqueous sample containing diethyldithiocarbamate complexes of metal ions. For a sample volume of 10 mL, enrichment factors of 277, 270 and 300 and detection limits of 1.2, 1.1 and 1 ng L-1 for nickel, cobalt and copper were obtained, respectively. The method was applied to the extraction and determination of these metals in different water samples.

Production of a bioherbicide agent in liquid and solid medium and in a biphasic cultivation system

The use of fungi in weeds control programs depends upon the conidia production in large scale. Therefore, this study aimed to evaluate liquid and solid culture media and the cultivation by biphasic system for the conidia production of Bipolaris euphorbiae Muchovej & Carvalho a specific pathogen of Euphorbia heterophylla. The liquid media were obtained from agro-industrial waste or by-products, and the solid media were prepared with mixtures of grains and grain derivatives. The liquid medium made with sugar cane molasses stood out from the others because it provided great sporulation (23 x 10(4) conidia mL-1 of medium), conidial viability (99.7%), and formation of mycelial fungal biomass (1.26 g 100 mL-1 of medium). On solid media conidial production was markedly higher than in liquid media, especially the medium composed by a blend of sorghum grain (40%) and soybean hulls (60%) where the fungus produced 2.3 x 10(7) conidia g-1 of medium. The cultivation of B. euphorbiae in biphasic system not promoted a significant increase in the production of conidia. The solid media were more effective for the mass production of fungus and mixtures of grains and derivatives were effective for increasing conidia production.

Vitaminas lipossolúveis em alimentos: uma abordagem analítica

This study concerns certain problems inherent to the determination of fat-soluble vitamins in food, from extraction methods to identification and quantification. The discussion involves the main official and unofficial extraction methods coupled with spectrophotometric and HPLC techniques in which vitamins samples are obtained through liquid-liquid-solid and liquid-liquid-solid-solid extraction, indispensable to the analytical separation of different chemical compounds with vitamin functions. A saponification stage, possibly coupled with supercritical fluid extraction appears to be mandatory in the determination of vitamins A and E in their alcoholic forms. Alternative identification and quantification procedures are outlined: biological and chemical assays, analytical separations by HPLC (normal and reversed-phase), UV detection (all fat-soluble vitamins) and fluorescence detection (retinoids and tocopherols). Automation from sample preparation to quantification stages increases the data acquisition rate.

Ultra-trace monitoring of copper in environmental and biological samples by inductively coupled plasma atomic emission spectrometry after separation and preconcentration by using octadecyl silica membrane disks modified by a new schiff's base

Ultra-trace amounts of Cu(II) were separated and preconcentrated by solid phase extraction on octadecyl-bonded silica membrane disks modified with a new Schiff,s base (Bis- (2-Hydroxyacetophenone) -2,2-dimethyl-1,3-propanediimine) (SBTD) followed by elution and inductively coupled plasma atomic emission spectrometric detection. The method was applied as a separation and detection method for copper(II) in environmental and biological samples. Extraction efficiency and the influence of sample matrix, flow rate, pH, and type and minimum amount of stripping acid were investigated. The concentration factor and detection limit of the proposed method are 500 and 12.5 pg mL-1, respectively.

Solid phase extraction of iron and lead in environmental matrices on amberlite xad-1180/pv

A solid phase extraction procedure using Amberlite XAD-1180/Pyrocatechol violet (PV) chelating resin for the determination of iron and lead ions in various environmental samples was established. The procedure is based on the sorption of lead(II) and iron(III) ions onto the resin at pH 9, followed by elution with 1 mol/L HNO3 and determination by flame atomic absorption spectrometry. The influence of alkaline, earth alkaline and some transition metals, as interferents, are discussed. The recoveries for the spiked analytes were greater than 95%. The detection limits for lead and iron by FAAS were 0.37 µg/L and 0.20 µg/L, respectively. Validation of the method described here was performed by using three certified reference materials (SRM 1515 Apple Leaves, SRM 2711 Montana Soil and NRCC-SLRS-4 Riverine Water). The procedure was successfully applied to natural waters and human hair.

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.

Um espalhador de baixo custo de fase estacionária em placas para cromatografia em camada delgada

Chromatography is a means of separating mixtures into their several components. TLC, mainly a liquid/solid process, is one of the separation techniques most often used. It is indispensable in laboratories dealing with natural products, organic and analytical chemistry. Commercial chromatography plates are offered at relatively high cost. In this work the construction of a hand-operated plate coater of stationary phases of low cost and good reproducibility is described to be used in teaching laboratories and research.