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ABSTRACT: This study proposes a FRAP assay adapted to FIA system with a merging zones configuration. The FIA system conditions were optimised with the response surface methodology using the central composite rotatable design. The optimisation parameters studied were: the carrier flow rate, the lengths of the sample and reagent loops, and reactor length. The conditions selected in accordance with the results were: carrier flow rate of 1.00ml/min, length of the loops 18.2cm and length of the reaction coil 210.1cm. The detection and quantification limits were, respectively, 28.6 and 86.8μmol/l Fe(2+), and the precision was 1.27%. The proposed method had an analytical frequency of 30samples/h and about 95% less volume of FRAP reagent was consumed. The FRAP assay adapted to the FIA system under the optimised conditions was utilised to determine the antioxidant activity of tea samples.
Food Chemistry 05/2013; 138(1):574-80. · 3.65 Impact Factor
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ABSTRACT: Activated carbons were prepared from flamboyant pods by NaOH activation at three different NaOH:char ratios: 1:1 (AC-1), 2:1 (AC-2), and 3:1 (AC-3). The properties of these carbons, including BET surface area, pore volume, pore size distribution, and pore diameter, were characterized from N(2) adsorption isotherms. The activated carbons obtained were essentially microporous and had BET surface area ranging from 303 to 2463 m(2) g(-1).(13)C (CP/MAS and MAS) solid-state NMR shows that the lignocellulosic structures were completely transformed into a polycyclic material after activation process, thermogravimetry shows a high thermal resistance, Boehm titration and Fourier-transform infrared spectroscopy allowed characterizing the presence of functional groups on the surface of activated carbons. Scanning electron microscopy images showed a high pore development. The experimental results indicated the potential use of flamboyant pods as a precursor material in the preparation of activated carbon.
Journal of Environmental Management 01/2011; 92(1):178-84. · 3.24 Impact Factor
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ABSTRACT: A first-order derivative spectrophotometric method for the simultaneous determination of three textile dyes, Procion Yellow HE4R, Procion Red HE7B and Remazol Black 5 (RB5), has been developed. The effects of pH, heating and ionic strength of the solution on the absorption spectra of the dyes were investigated. The wavelengths selected for the measures of the derivative signals of HE4R (395 nm), HE7B (604 nm) and RB5 (659 nm) presented these coefficients of linear correlation: 0.9978, 0.9992 and 0.9999, and these detection limits: 0.180, 0.317 and 0.0233 mg L(-1), respectively. The reliability and reproducibility of the method were tested and showed recovery values of 95.7 to 109%. The proposed method was applied for the determination of dyes in binary and ternary mixtures of textile effluents and showed an estimate of the loss of dyes for the effluents between 6.67 and 28.9%.
Analytical Sciences 05/2009; 25(4):487-92. · 1.25 Impact Factor
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ABSTRACT: A new spectrophotometric method involving flow injection analysis and textile dye aggregation effect is proposed. The method is based on the aggregation effect of Blue Procion HEGN at pH 3, which relocates its maximum absorption wavelength from 620 to 776 nm, avoiding the interference of other blue textile dyes. For this task, a simple and robust flow injection system was designed, which became a very stable analytical method. When the system was applied to Blue Procion determination in effluent of textile industry, precise results were observed (RSD < 2% within 1.0 and 5.0 mg l(-1) HEGN). The analytical frequency was 80 measurements per hour; the analytical curve was linear from 1.0 to 5.0 mg l(-1) HEGN; the detection limit considering three times the standard deviation of the blank solution (n = 10) was estimated as 0.03 mg l(-1) HEGN; and recoveries between 95% and 105% were found. The system consumes 20 mg of sodium citrate and 125 microl of the sample per determination. No baseline drift was observed during extended (5 h) operation periods.
Analytical Sciences 03/2006; 22(3):445-8. · 1.25 Impact Factor
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ABSTRACT: A procedure involving bead-injection concept and sequential determination of copper and mercury ions in river-water samples is proposed. The method is based on the solid-phase extraction of both metal ions on the same beads surface (Chelex 100 resin) and in their subsequent reaction with the colorimetric reagents (APDC and Dithizone for copper and mercury ions, respectively). For this task, a resin mini-column is established in the optical path by the selection, introduction and trapping of a defined volume of the Chelex-100 resin beads suspension in the flow system. The passage of the sample solution through the resin mini-column promotes the sorption of Cu(II) ions and, making the APDC colorimetric reagent flows through the beads, the formation of the coloured complex on the solid phase surface occurs. The absorbance of the formed APDC-Cu complex is then monitored at 436nm and the spent beads are discarded. Packing another resin mini-column in the flow cell and repeating the concentration step it is possible to carried out the mercury determination by using Dithizone as reagent. The absorbance of the Dithizone-Hg complex is monitored at 500nm. After each measurement, the spent beads are wasted and a new portion of fresh one is trapped in the system, letting it ready for the next measurement. The bead injection system is versatile and can be used to concentrate different sample volumes, which permits the determination of a wide range of copper and mercury ions concentrations. When the sample-selected volumes are 100 and 1000mul the analytical ranges were 5.0 up to 500.0mugl(-1) and 2.5 up to 30.0mugl(-1) for Cu(II) and Hg(II) ions, respectively. Under these conditions, the detection limit was estimated as 0.63 and 0.25mugl(-1) for copper and mercury ions determination. The system consumes 2mg of Chelex 100 resin beads, 0.20mg of APDC or 1.25mg of Dithizone per determination and the traditional organic solvent extraction methodology, normally used in connection with APDC and Dithizone reagents, is not used here which permits to classify the present method as green.
Talanta 12/2004; 64(4):993-9. · 3.79 Impact Factor
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ABSTRACT: The conditions for the preparation of activated carbon from flamboyant pods treated with NaOH were optimized through response surface methodology (RSM) and central composite rotatable design (CCRD). The effects of the activation temperature, activation time, and impregnation ratio were studied from the BET surface area, micropore volume, and yield results. The results showed that the activation temperature and the impregnation ratio are the factors that most influence the activated carbon production. Activation temperature of 761.70 °C, activation time of 0.86 h, and impregnation ratio (NaOH:char) of 3.46 led to BET surface area, micropore volume, and yield values of 2854 m2 g−1, 1.44 cm3 g−1, and 10.80%, respectively. Porosity parameters and scanning electron microscopy were used to investigate the activated carbon obtained under optimal conditions.
Chemical Engineering Journal. 162(1):43-50.
