Neste trabalho são descritos e comparados dois métodos espectrofotométricos para análise de catecol (o-hidroxifenol) em Paullinea cupana var. sorbilis, popularmente conhecido como guaraná. As amostras de sementes trituradas foram extraídas com etanol 97% v/v e as soluções tratadas com p-aminofenol em meio etanólico alcalino ou m-aminofenol e metaperiodato de sódio em solução tampão (pH 3.0). A absorbância foi medida a 586 nm e 520 nm respectivamente. Quatro produtos comerciais diferentes foram analisados e os resultados foram comparados com aqueles obtidos com m-aminofenol. Apesar da boa qualidade das curvas de calibração, nos dois métodos houve interferência da matriz, o que foi contornado usando-se o método da adição de padrão. A comparação entre os resultados obtidos pelos dois métodos, usando o teste estatístico t de Student, mostrou que não há diferenças significantes para um nível de confiança de 95%.In this article are described and compared two spectrophotometric methods for the analysis of catechol (o-hydroxyphenol) in Paullinea cupana var. sorbilis, popularly known as guaraná. The pounded seed samples were extracted with ethanol 97% v/v and the solutions were treated with p-aminophenol in alkaline ethanolic medium or m-aminophenol and sodium metaperiodate in buffered aqueous solution (pH 3.0). The absorbance was measured at 586 nm and 520 nm respectively. Four different commercial products were analyzed and the results were compared with those obtained with the m-aminophenol method. Despite the good quality of the calibration curves, in the two methods the interference of the matrix was observed. This problem was settled using the standard addition method. Comparison between the results obtained by the two methods, using the statistical Student's t-test, showed that there is no significant difference at the 95% confidence level.
In this paper, a low-cost and versatile lab-made photoreactor was constructed for the preparation of nanomaterials such as gold nanoparticles and reduced graphene oxide. The power of the lab-made photoreactor can be easily adjusted according to the number of lamps turned on. Moreover, the lab-made photoreactor allows the utilization of different sources of irradiation with distinct wavelengths. Performance tests for production of gold nanoparticles showed reproducibility and equal efficiency as compared to the literature. Also, the photoreactor powered with UV-A and UV-C as sources of irradiation can be used for modulation of the reduction degree of graphene oxide.
Biodiesel degrades due to oxidative processes, causing a decrease in its quality. In the present work, it has been clearly shown that the incidence of ultraviolet radiation on biodiesels obtained from soy, canola, linseed and microalgae oils initiate oxidative processes which lead to the decrease in the induction period (IP) of the fuel. The influence of the residual water content of the same biodiesels on the oxidation process was also investigated with and without the incidence of ultraviolet radiation. Between 190 and 850 ppm of water in the biodiesel and without UV irradiation, no significant change in the IP values was observed under the experimental conditions. Keywords: biodiesel, oxidative stability, photo-oxidation, residual water IntroductionBiodiesel is a biofuel derived from renewable sources such as vegetable oils and animal fats. It presents physicochemical characteristics similar to that of petrodiesel and can therefore be directly used in diesel engines. Because biodiesel is produced from renewable and biodegradable raw materials, it presents some advantages over petrodiesel, for example, the absence of sulfur in emissions, a high flash point, and good lubricity. 1,2 Biodiesel is composed of a mixture of alkyl esters, usually methyl or ethyl derivatives, obtained through transesterification reactions of vegetable oils and animal fats with methanol or ethanol in the presence of a catalyst.Oxidation reactions of biodiesel can occur on account of various factors, such as high unsaturation and total number and position of allylic and bis-allylic carbons that are adjacent to the double bonds of the molecules of alkyl esters, exposure to light, temperature, presence of transition metals, and exposure to oxygen. [3][4][5] It was also reported that hydrolysis reactions can occur depending on the environmental humidity or even on the humidity present in the storage tanks. Residual water is particularly problematic because it can hydrolyze the biodiesel, producing free fatty acids and alcohol and increasing the acid number of biodiesel. 6Similar to lipids, the oxidation of biodiesel occurs mainly through two processes called auto-oxidation and photo-oxidation. Auto-oxidation is the main cause of the oxidation of biodiesel. It involves the formation of free radicals and can be summarized in three steps called initiation, propagation, and termination, as schematized in Figure 1. 7 In the first phase, known as the induction or initiation period, the initial formation of free radicals occurs. In the second phase, known as propagation, the formation of a great quantity of peroxides and hydroperoxides occurs. Finally, the termination step occurs, forming high concentrations of degradation products, such as alcohols, aldehydes, ketones, organic acids, and polymers, whose presence changes the properties of the biodiesel. Vol. 28, No. 4, 2017 Another type of oxidation reaction that biodiesel can undergo is the photo-oxidation. Free radicals, which are known as initiators of oxidation processes, are formed as a...
Oxidative stability parameters (OSP), acid value (AV), water content (W), and the metallic copper corrosion rate in biodiesels obtained from eight different vegetable oils were determined. Simple and multiple linear regression models were constructed to explain the influence of the OSP, AV and W variables on the corrosion rate. The corrosion rate was lower in biodiesel with less oxidative stability because, instead of reacting with copper, O 2 reacted preferentially with the unsaturated fatty acid methyl esters (FAME) that could act as "sacrificial molecules" to protect the copper against corrosion. Therefore, the corrosion rate was strongly related to the FAME composition. The AV was an important parameter in the corrosion process because free acids react with passivating agents, increasing the corrosion rate. The predictive capacity of W for corrosion rate was statistically insignificant, although water condensed on a copper surface causes corrosion.
A flow injection method for the quantitative analysis of vancomycin hydrochloride, C66H75Cl2N9O24.HCl (HVCM), based on the reaction with copper (II) ions, is presented. HVCM forms a lilac-blue complex with copper ions at pH≅4.5 in aqueous solutions, with maximum absorption at 555 nm. The detection limit was estimated to be about 8.5×10-5 mol L-1; the quantitation limit is about 2.5×10-4 mol L-1 and about 30 determinations can be performed in an hour. The accuracy of the method was tested through recovery procedures in presence of four different excipients, in the proportion 1:1 w/w. The results were compared with those obtained with the batch spectrophotometric and with the HPLC methods. Statistical comparison was done using the Student's procedure. Complete agreement was found at a 0.95 significance level between the proposed flow injection and the batch spectrophotometric methods, which present similar precision (RSD: 2.1 % vs. 1.9%).
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