Vitor C. Almeida

Preparation and characterization of activated carbon from a new raw lignocellulosic material: Flamboyant (Delonix regia) pods

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.

Evaluation of solvent effect on the extraction of phenolic compounds and antioxidant capacities from the berries: application of principal component analysis

BackgroundThis study evaluated the effect of the solvent on the extraction of antioxidant compounds from black mulberry (Morus nigra), blackberry (Rubus ulmifolius) and strawberry (Fragaria x ananassa). Different extracts of each berry were evaluated from the determination of total phenolic content, anthocyanin content and antioxidant capacity, and data were applied to the principal component analysis (PCA) to gain an overview of the effect of the solvent in extraction method.ResultsFor all the berries analyzed, acetone/water (70/30, v/v) solvent mixture was more efficient solvent in the extracting of phenolic compounds, and methanol/water/acetic acid (70/29.5/0.5, v/v/v) showed the best values for anthocyanin content. Mixtures of ethanol/water (50/50, v/v), acetone water/acetic acid (70/29.5/0.5, v/v/v) and acetone/water (50/50, v/v) presented the highest antioxidant capacities for black mulberries, blackberries and strawberries, respectively.ConclusionAntioxidants extractions are extremely affected by the solvent combination used. In addition, the obtained extracts with the organic solvent-water mixtures were distinguished from the extracts obtained with pure organic solvents, through the PCA analysis.

Exploiting the bead injection concept for sequential determination of copper and mercury ions in river-water samples

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.

The antioxidant activity of teas measured by the FRAP method adapted to the FIA system: optimising the conditions using the response surface methodology.

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 1.00 ml/min, length of the loops 18.2 cm and length of the reaction coil 210.1 cm. The detection and quantification limits were, respectively, 28.6 and 86.8 μmol/l Fe(2+), and the precision was 1.27%. The proposed method had an analytical frequency of 30 samples/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.

Evolutive follow-up of the photocatalytic degradation of real textile effluents in TiO2 and TiO2/H2O2 systems and their toxic effects on Lactuca sativa seedlings

Textile industry wastes raise a great concern due to their strong coloration and toxicity. The objective of the present work was to characterize the degradation and mineralization of textile effluents by advanced oxidative processes using either TiO2 or TiO2/H2O2 association and to monitor the toxicity of the products formed during 6 h irradiation in relation to that of the in natura effluent. The results obtained demonstrated that the TiO2/H2O2 association was more efficient in the mineralization of textile effluents than TiO2 alone, with high mineralized ion concentrations (NH4+, NO3-, and SO42-) and significant organic matter reduction rates (represented by the COD and TOC). The toxicity of the degradation products to lettuce seeds (Lactuca sativa) was not significant, since percent germination was not significantly affected and neither was root and sprout percent growth. However, while the TiO2/H2O2 association was more toxic in the first hours of irradiation and less so in the end of the 6 h irradiation, the toxicity of TiO2 increased only slightly in the end of the experiments. Comparatively, the photogenerated products of both the TiO2 and the TiO2/H2O2 association were less toxic than the in natura effluent.

Adsorption of caffeine on mesoporous activated carbon fibers prepared from pineapple plant leaves

The present work reports the preparation of activated carbon fibers (ACFs) from pineapple plant leaves, and its application on caffeine (CFN) removal from aqueous solution. The preparation procedure was carried out using the H3PO4 as activating agent and slow pyrolysis under N2 atmosphere. The characterization of materials was performed from the N2 adsorption and desorption isotherms, scanning electron microscopy (SEM), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Raman spectroscopy, Boehm titration and pHpzc method. ACFs showed high BET surface area value (SBET = 1031m2 g-1), well-developed mesoporous structure (mesopore volume of 1.27cm³ g-1) and pores with average diameter (DM) of 5.87nm. Additionally, ACFs showed features of fibrous material with predominance of acid groups on its surface. Adsorption studies indicated that the pseudo-second order kinetic and Langmuir isotherm models were that best fitted to the experimental data. The monolayer adsorption capacity was found to be 155.50mgg-1. thermodynamic studies revealed that adsorption process is spontaneous, exothermic and occurs preferably via physisorption. The pineapple leaves are an efficient precursor for preparation of ACFs, which were successful applied as adsorbent material for removal of caffeine from the aqueous solutions.

Effect of dietary replacement of sunflower oil with perilla oil on the absolute fatty acid composition in Nile tilapia (GIFT)

This study evaluated the effect of the dietary replacement of sunflower oil with perilla oil in Nile tilapia (GIFT strain) at 0, 10, 20 and 30 days. There was an increase in total omega 3 fatty acids (n-3) in muscle tissue (from 63.6 to 181.5 mg g(-1)) and a decrease in total concentration of omega 6 fatty acids (n-6) ranging between 255.6 and 196.1 mgg(-1). Amongst the n-3 fatty acids, the concentrations of alpha-linolenic acid (18:3n-3) and docosahexaenoic acid (20:6n-3) increased by 9.4 and 1.9 times, respectively, after 30 days for the perilla oil-enriched diet. The n-6/n-3, polyunsaturated and saturated fatty acids (PUFA/SFA), and polyunsaturated and monounsaturated fatty acids (PUFA/MUFA) ratios tended to stabilize after 20 days under the perilla oil-enriched diet. Incorporation of perilla oil as a lipid source in the diet of tilapia for 20 or 30 days resulted in significant changes in the fatty acid composition of the fish muscle tissue, contributing to increase its nutritional value.

Determinação de cobre, alumínio e ferro em solos derivados do basalto através de extrações seqüenciais

Copper, aluminum and iron concentrations were determined in four geochemical fractions of three different basaltic soils from the northwest region of the Parana State, Brazil. The fractions examined were the reducible manganese dioxide and amorphous iron oxide, crystaline iron oxide, organic and residual. Metal concentrations were determined in the extracts by flame atomic absorption spectrophotometry. High Fe concentrations were extracted from the crystalline iron oxide (>20%), as well as the amorphous iron oxide (>12%). Copper was extracted from the amorphous and crystalline iron oxides in the range 5 to 12%, but low concentrations were bound to organic matter. Low concentrations of aluminum were extracted (<8%) from the amorphous and crystaline iron oxides, and organic matter. High concentrations of aluminum were found in the residual fraction.

Toxic effects of dietary of Al3+ ions in tilapias (Oreochromis niloticus) and protective effect of Zn2+ ion

The lethal effects of aluminum ion (Al3+) in tilapia (Oreochromis niloticus) raised in concrete tanks were investigated. Tilapias were fed daily with commercial feed enriched with known concentrations of Al3+ and analyzed by differential pulse anodic stripping voltammetry (DPASV). The concentrations of Al3+ in feces, water, muscle tissue, viscera, and heads were determined every 3 months for a period of 365 days. The Tilapia head was the most affected tissue by Al3+. In general, Al3+ bioaccumulation reached the lethal dose (LD50) after 335 days of experiment as follows: 34.9 mg kg−1 (muscle tissue), 88.2 mg kg−1 (viscera), and 126.9 mg kg−1 (head without gills). After determining Cu2+, Zn2+, and Ca2+ by absorption spectrometry, a decrease in the Ca2+ concentration was noted in the head during the experimental period. These observations were associated with the occurrence of a decalcification in the bone tissue in the presence of Al3+. In contrast, it was found that Zn2+ ions may act as a protective agent against Al3+-induced contamination.

Determination of Vitamins A and E Exploiting Cloud Point Extraction and Micellar Liquid Chromatography

Cloud point extraction and micellar chromatographic methods were developed for determination of vitamins A and E. The stationary phase was C18 and the mobile phase was 3.00% (w/v) SDS, 15.0% (v/v) butyl alcohol and 0.02 mol L−1 phosphate buffer solution at pH 7.0. The retention times for vitamins A and E were 9.6 and 13.0, respectively. The extraction solution was 100 mmol L−1 Triton X-100, 650 mg NaCl and 1.0% ascorbic acid at 70°C for 30 min. The method is precise (r.s.d. < 7%), the linear range was from 5.0 up to 360.0 mg L−1 for both vitamins. Recovery test showed recuperation between 90.2 and 99.2%, and LOD and LOQ of 0.234 and 0.108 mg L−1, 0.780 and 0.360 mg L−1 to vitamins A and E were found.