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URI permanente para esta coleçãohttps://locus.ufv.br/handle/123456789/11800

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    A green and sensitive method to determine phenols in water and wastewater samples using an aqueous two-phase system
    (Talanta, 2009-09-04) Rodrigues, Guilherme Dias; Lemos, Leandro Rodrigues de; Silva, Luis Henrique Mendes da; Silva, Maria do Carmo Hespanhol da; Minim, Luis Antonio; Coimbra, Jane Sélia dos Reis
    A greener and more sensitive spectrophotometric procedure has been developed for the determination of phenol and o-cresol that exploits an aqueous two-phase system (ATPS) using a liquid–liquid extraction technique. An ATPS is formed mostly by water and does not require organic solvent. Other ATPS components used in this study were the polymer, polyethylene oxide, and some salts (i.e., Li2SO4, Na2SO4 or K2HPO4 + KOH). The method is based on the reaction between phenol, sodium nitroprusside (NPS) and hydroxylamine hydrochloride (HL) in an alkaline medium (pH 12.0), producing the complex anion [Fe2(CN)10]^10− that spontaneously concentrates in the top phase of the system. The linear range was 1.50–500 μg kg^−1 (R ≥ 0.9997; n = 8) with coefficients of variation equal to 0.38% for phenol and 0.30% for o-cresol (n = 5). The method yielded limits of detection (LODs) of 1.27 and 1.88 μg kg^−1 and limits of quantification (LOQs) of 4.22 and 6.28 μg kg^−1 for phenol and o-cresol, respectively. Recoveries between 95.7% and 107% were obtained for the determination of phenol in natural water and wastewater samples. In addition, excellent agreement was observed between this new ATPS method and the standard 4-aminoantipyrine (4-AAP) method.
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    Aqueous two-phase systems: An efficient, environmentally safe and economically viable method for purification of natural dye carmine
    (Tecnologia de Alimentos, 2009-11-09) Mageste, Aparecida Barbosa; Lemos, Leandro Rodrigues de; Ferreira, Guilherme Max Dias; Silva, Maria do Carmo Hespanhol da; Silva, Luis Henrique Mendes da; Bonomo, Renata Cristina Ferreira; Minim, Luis Antonio
    Partition of the natural dye carmine has been studied in aqueous two-phase systems prepared by mixing aqueous solutions of polymer or copolymer with aqueous salt solutions (Na2SO4 and Li2SO4). The carmine dye partition coefficient was investigated as a function of system pH, polymer molar mass, hydrophobicity, system tie-line length and nature of the electrolyte. It has been observed that the carmine partition coefficient is highly dependent on the electrolyte nature and pH of the system, reaching values as high as 300, indicating the high potential of the two-phase extraction with ATPS in the purification of carmine dye. The partition relative order was Li2SO4 ≫ Na2SO4. Carmine molecules were concentrated in the polymer-rich phase, indicating an enthalpic specific interaction between carmine and the pseudopolycation, which is formed by cation adsorption along the macromolecule chain. When the enthalpic carmine–pseudopolycation interaction decreases, entropic forces dominate the natural dye-transfer process, and the carmine partitioning coefficient decreases. The optimization of the extraction process was obtained by a central composite face-centered (CCF) design. The CCF design was used to evaluate the influence of Li2SO4 and PEO 1500 concentration and of the pH on the partition coefficient of carmine. The conditions that maximize the partition of carmine into the top phase were determined to be high concentrations of PEO and Li2SO4 and low pH values within the ranges studied.