941 resultados para Method of extraction


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A new method to extract MOSFET's threshold voltage VT by measurement of the gate-to-substrate capacitance C-gb of the transistor is presented. Unlike existing extraction methods based on I-V data, the measurement of C-gb does not require de drain current to now between drain and source thus eliminating the effects of source and drain series resistance R-S/D, and at the same time, retains a symmetrical potential profile across the channel. Experimental and simulation results on devices with different sizes are presented to justify the proposed method.

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A new cloud point extraction (CPE) method was developed for the separation and preconcentration of copper (II) prior to spectrophotometric analysis. For this purpose, 1-(2,4-dimethylphenyl) azonapthalen-2-ol (Sudan II) was used as a chelating agent and the solution pH was adjusted to 10.0 with borate buffer. Polyethylene glycol tert-octylphenyl ether (Triton X-114) was used as an extracting agent in the presence of sodium dodecylsulphate (SDS). After phase separation, based on the cloud point of the mixture, the surfactant-rich phase was diluted with acetone, and the enriched analyte was spectrophotometrically determined at 537 nm. The variables affecting CPE efficiency were optimized. The calibration curve was linear within the range 0.285-20 µg L-1 with a detection limit of 0.085 µg L-1. The method was successfully applied to the quantification of copper in different beverage samples.

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Climatic impacts of energy-peat extraction are of increasing concern due to EU emissions trading requirements. A new excavation-drier peat extraction method has been developed to reduce the climatic impact and increase the efficiency of peat extraction. To quantify and compare the soil GHG fluxes of the excavation drier and the traditional milling methods, as well as the areas from which the energy peat is planned to be extracted in the future (extraction reserve area types), soil CO2, CH4 and N2O fluxes were measured during 2006–2007 at three sites in Finland. Within each site, fluxes were measured from drained extraction reserve areas, extraction fields and stockpiles of both methods and additionally from the biomass driers of the excavation-drier method. The Life Cycle Assessment (LCA), described at a principal level in ISO Standards 14040:2006 and 14044:2006, was used to assess the long-term (100 years) climatic impact from peatland utilisation with respect to land use and energy production chains where utilisation of coal was replaced with peat. Coal was used as a reference since in many cases peat and coal can replace each other in same power plants. According to this study, the peat extraction method used was of lesser significance than the extraction reserve area type in regards to the climatic impact. However, the excavation-drier method seems to cause a slightly reduced climatic impact as compared with the prevailing milling method.

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In metallurgical practice today some of the relatively rare metal Indium is recovered as a by-product from the ores of other metals. Indium is a soft, silvery—white metal belonging to the third group of the periodic classification. It is situated just above tin in the electrochemical series.

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Despite the considerable environmental importance of mercury (Hg), given its high toxicity and ability to contaminate large areas via atmospheric deposition, little is known about its activity in soils, especially tropical soils, in comparison with other heavy metals. This lack of information about Hg arises because analytical methods for determination of Hg are more laborious and expensive compared to methods for other heavy metals. The situation is even more precarious regarding speciation of Hg in soils since sequential extraction methods are also inefficient for this metal. The aim of this paper is to present a technique of thermal desorption associated with atomic absorption spectrometry, TDAAS, as an efficient tool for quantitative determination of Hg in soils. The method consists of the release of Hg by heating, followed by its quantification by atomic absorption spectrometry. It was developed by constructing calibration curves in different soil samples based on increasing volumes of standard Hg2+ solutions. Performance, accuracy, precision, and quantification and detection limit parameters were evaluated. No matrix interference was detected. Certified reference samples and comparison with a Direct Mercury Analyzer, DMA (another highly recognized technique), were used in validation of the method, which proved to be accurate and precise.

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Lettuce is worldwide known as the most important vegetable. In this context, most farmers are searching new techniques for best quality products including hydropony. However, nitrate is of great concern, since it has a negative impact on human metabolism. The main objective of the present work was to evaluate the nitrate content of lettuce produced by conventional and hydroponic systems. The determination was conducted by ion chromatography and a new method of extraction was tested using microwave oven digestion. The results indicated that nitrate level produced in the conventional system was lower than in the hydroponic system.

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This paper describes the optimization of a multiresidue chromatographic analysis for the identification and quantification of 20 pesticides in bovine milk, including three carbamates, a carbamate oxime, six organophosphates, two strobilurins, a pyrethroid, an oxazolidinedione, an aryloxyphenoxypropionate acid/ester, a neonicotinoid, a dicarboximide, and three triazoles. The influences of different chromatographic columns and gradients were evaluated. Furthermore, four different extraction methods were evaluated; each utilized both different solvents, including ethyl acetate, methanol, and acetonitrile, and different workup steps. The best results were obtained by a modified QuEChERS method that lacked a workup step, and that included freezing the sample for 2 hours at -20 ºC. The results were satisfactory, yielding coefficients of variation of less than 20%, with the exception of the 50 µg L-1 sample of famoxadone, and recoveries between 70 and 120%, with the exception of acephate and bifenthrin; however, both analytes exhibited coefficients of variation of less than 20%.

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The objective of this study was to optimize and validate the solid-liquid extraction (ESL) technique for determination of picloram residues in soil samples. At the optimization stage, the optimal conditions for extraction of soil samples were determined using univariate analysis. Ratio soil/solution extraction, type and time of agitation, ionic strength and pH of extraction solution were evaluated. Based on the optimized parameters, the following method of extraction and analysis of picloram was developed: weigh 2.00 g of soil dried and sieved through a sieve mesh of 2.0 mm pore, add 20.0 mL of KCl concentration of 0.5 mol L-1, shake the bottle in the vortex for 10 seconds to form suspension and adjust to pH 7.00, with alkaline KOH 0.1 mol L-1. Homogenate the system in a shaker system for 60 minutes and then let it stand for 10 minutes. The bottles are centrifuged for 10 minutes at 3,500 rpm. After the settlement of the soil particles and cleaning of the supernatant extract, an aliquot is withdrawn and analyzed by high performance liquid chromatography. The optimized method was validated by determining the selectivity, linearity, detection and quantification limits, precision and accuracy. The ESL methodology was efficient for analysis of residues of the pesticides studied, with percentages of recovery above 90%. The limits of detection and quantification were 20.0 and 66.0 mg kg-1 soil for the PVA, and 40.0 and 132.0 mg kg-1 soil for the VLA. The coefficients of variation (CV) were equal to 2.32 and 2.69 for PVA and TH soils, respectively. The methodology resulted in low organic solvent consumption and cleaner extracts, as well as no purification steps for chromatographic analysis were required. The parameters evaluated in the validation process indicated that the ESL methodology is efficient for the extraction of picloram residues in soils, with low limits of detection and quantification.

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This study aims to optimize an alternative method of extraction of carrageenan without previous alkaline treatment and ethanol precipitation using Response Surface Methodology (RSM). In order to introduce an innovation in the isolation step, atomization drying was used reducing the time for obtaining dry carrageenan powder. The effects of extraction time and temperature on yield, gel strength, and viscosity were evaluated. Furthermore, the extracted material was submitted to structural analysis, by infrared spectroscopy and nuclear magnetic resonance spectroscopy (¹H-NMR), and chemical composition analysis. Results showed that the generated regression models adequately explained the data variation. Carrageenan yield and gel viscosity were influenced only by the extraction temperature. However, gel strength was influenced by both, extraction time and extraction temperature. Optimal extraction conditions were 74 ºC and 4 hours. In these conditions, the carrageenan extract properties determined by the polynomial model were 31.17%, 158.27 g.cm-2, and 29.5 cP for yield, gel strength, and viscosity, respectively, while under the experimental conditions they were 35.8 ± 4.68%, 112.50 ± 4.96 g.cm-2, and 16.01 ± 1.03 cP, respectively. The chemical composition, nuclear magnetic resonance spectroscopy, and infrared spectroscopy analyses showed that the crude carrageenan extracted is composed mainly of κ-carrageenan.

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Different extraction processes were employed to extract the polyphenolic compounds from pitanga (Eugenia uniflora L) leaves: a one-step process using water, ethanol or supercritical CO(2) as solvents, and a two-step process using supercritical CO(2) followed by either water or ethanol. The total polyphenolic compounds, total flavonoids and antioxidant activity were determined in all the extracts obtained. The process performance was evaluated with respect to three variables: global extraction yield, concentration and yield of both polyphenols and flavonoids in the extracts. For the one-step extraction, the results showed that the extraction yield increased with solvent polarity. For the two-step process, the results suggested that water was more efficient in extracting the phenolic compounds from E. uniflora when the matrix was previously extracted with scCO(2). With respect to the antioxidant activity, the ethanolic extracts obtained from both processes, using either the DPPH radical scavenging method or the beta-carotene bleaching method, presented high antioxidant activities. (C) 2010 Elsevier B.V. All rights reserved.

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Antioxidants are substances that may protect cells from the damage caused by unstable molecules known as free radicals. The capacity of natural antioxidant from phytochemical has increase attention from researchers and public. However, the extraction process is affecting the activity and the bioavailability of bioactive compounds. The Solanum lycocarpum is a plant of the Brazilian “cerrado”, popularly used as a hypoglycemic, hypocholesterolemic and control of metabolic diseases. Its effects are attributed to the presence of several glycoalkaloids (solamargine, solasonina) and solasodine. Therefore, the purpose of this communication was, investigate the optimization of extraction condition and evaluation of antioxidant activity from fruits of Solanum lycocarpum. The extracts were obtained using different solvent systems, i.e., water, 50% ethanol, ethanol absolute and ethyl ether (1:10 and 1:20) and different extraction processes: maceration with constant agitation at room temperature, maceration with constant agitation and heating at 30°C and ultrasound. The extracts were characterized by the amount of material extracted (1, 6 and 24 h) and the action of antioxidant activity by DPPH method. The results showed that the polar solvent (50% ethanol) and extractive process maceration with agitation to ambient temperature showed higher contents of extractable of fruits of S. lycocarpum (3.4 g %) and also showed higher antioxidant activity (88.57±2.41% de inhibition). This action whether the presence of glycoalkaloids (solamargine, solasonine and solasodine) in fruits S. lycocarpum which are polar compounds and may explain this increased antioxidant action of this extract.

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Seaweeds are photosynthetic organisms important to their ecosystem and constitute a source of compounds with several different applications in the pharmaceutical, cosmetic and biotechnology industries, such as triacylglycerols, which can be converted to fatty acid methyl esters that make up biodiesel, an alternative source of fuel applied in economic important areas. This study evaluates the fatty acid profiles and concentrations of three Brazilian seaweed species, Hypnea musciformis (Wulfen) J.V. Lamouroux (Rhodophya), Sargassum cymosum C. Agardh (Heterokontophyta), and Ulva lactuca L. (Chlorophyta), comparing three extraction methods (Bligh & Dyer - B&D; AOAC Official Methods - AOM; and extraction with methanol and ultrasound - EMU) and two transesterification methods (7% BF3 in methanol - BF3; and 5% HCl in methanol - HCl). The fatty acid contents of the three species of seaweeds were significantly different when extracted and transesterified by the different methods. Moreover, the best method for one species was not the same for the other species. The best extraction and transesterification methods for H. musciformis, S. cymosum and U. lactuca were, respectively, AOM-HCl, B&D-BF3 and B&D-BF3/B&D-HCl. These results point to a matrix effect and the method used for the analysis of the fatty acid content of different organisms should be selected carefully.

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An easily implemented extension of the standard response method of tidal analysis is outlined. The modification improves the extraction of both the steady and the tidal components from problematic time series by calculating tidal response weights uncontaminated by missing or anomalous data. Examples of time series containing data gaps and anomalous events are analyzed to demonstrate the applicability and advantage of the proposed method.

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Evaluation of the quality of the environment is essential for human wellness as pollutants in trace amounts can cause serious health problem. Nitrosamines are a group of compounds that are considered potential carcinogens and can be found in drinking water (as disinfection byproducts), foods, beverages and cosmetics. To monitor the level of these compounds to minimize daily intakes, fast and reliable analytical techniques are required. As these compounds are relatively highly polar, extraction and enrichment from environmental samples (aqueous) are challenging. Also, the trend of analytical techniques toward the reduction of sample size and minimization of organic solvent use demands new methods of analysis. In light of fulfilling these requirements, a new method of online preconcentration tailored to an electrokinetic chromatography is introduced. In this method, electroosmotic flow (EOF) was suppressed to increase the interaction time between analyte and micellar phase, therefore the only force to mobilize the neutral analytes is the interaction of analyte with moving micelles. In absence of EOF, polarity of applied potential was switched (negative or positive) to force (anionic or cationic) micelles to move toward the detector. To avoid the excessive band broadening due to longer analysis time caused by slow moving micelles, auxiliary pressure was introduced to boost the micelle movement toward the detector using an in house designed and built apparatus. Applying the external auxiliary pressure significantly reduced the analysis times without compromising separation efficiency. Parameters, such as type of surfactants, composition of background electrolyte (BGE), type of capillary, matrix effect, organic modifiers, etc., were evaluated in optimization of the method. The enrichment factors for targeted analytes were impressive, particularly; cationic surfactants were shown to be suitable for analysis of nitrosamines due to their ability to act as hydrogen bond donors. Ammonium perfluorooctanoate (APFO) also showed remarkable results in term of peak shapes and number of theoretical plates. It was shown that the separation results were best when a high conductivity sample was paired with a BGE of lower conductivity. Using higher surfactant concentrations (up to 200 mM SDS) than usual (50 mM SDS) for micellar electrokinetic chromatography (MEKC) improved the sweeping. A new method for micro-extraction and enrichment of highly polar neutral analytes (N-Nitrosamines in particular) based on three-phase drop micro-extraction was introduced and its performance studied. In this method, a new device using some easy-to-find components was fabricated and its operation and application demonstrated. Compared to conventional extraction methods (liquid-liquid extraction), consumption of organic solvents and operation times were significantly lower.