Doehlert matrix for optimisation of procedure for determination of nickel in saline oil-refinery effluents by use of flame atomic absorption spectrometry after preconcentration by cloud-point extraction

This paper proposes a preconcentration procedure for determination of nickel in saline aqueous waste samples by flame atomic absorption spectrometry (FAAS). It is based on cloud-point extraction of nickel(II) ions as 2-(5-bromo-2-pyridylazo)-5-diethilaminophenol (Br-PADAP) complexes using octylphenoxypolyethoxyethanol (Triton X-114) as surfactant. The optimisation step was performed using a four-variable Doehlert design, involving the factors centrifugation time (CT) of system after addition of surfactant, solution pH, methanol volume (MV) added at micellar phase, and buffer concentration (BC). The analytical response used was absorbance, after volume correction. Using the established experimental conditions in the optimisation step the procedure enables nickel determination with a detection limit (3 delta/ S) of 0.2 microg L(-1), quantification limit (10 delta/ S) of 0.7 microg L(-1), and precision, calculated as relative standard deviation ( RSD) of 4.7 ( n=8) and 3.5% ( n=8) for nickel concentration of 1 and 5 microg L(-1), respectively. The preconcentration factor, determined from the ratio of the slopes of the analytical curves with and without preconcentration, is 74. The recovery achieved for nickel determination in the presence of several cations demonstrated that this procedure could be applied for analysis of water samples. The robustness was checked by using saturated fractional factorial designs, centred on the established experimental conditions in the optimisation step. The results of these tests demonstrated that the variables centrifugation time and buffer concentration are robust for modification by 10% and that solution pH and methanol volume are robust for 5%. Accuracy was evaluated by using the certified material reference SLEW-3 estuarine water for trace metals. The procedure was used for determination of nickel in saline effluents from oil refinery samples. Recovery results (95-104%) indicate that the procedure has satisfactory accuracy for nickel determination in these samples.     

Confluent Heun functions and the physics of black holes: Resonant frequencies,Hawking radiation and scattering of scalar waves

We apply the confluent Heun functions to study the resonant frequencies (quasispectrum), the Hawking radiation and the scattering process of scalar waves, in a class of spacetimes, namely, the ones generated by a Kerr–Newman–Kasuya spacetime (dyon black hole) and a Reissner–Nordström black hole surrounded by a magnetic field (Ernst spacetime). In both spacetimes, the solutions for the angular and radial parts of the corresponding Klein–Gordon equations are obtained exactly, for massive and massless fields, respectively. The special cases of Kerr and Schwarzschild black holes are analyzed and the solutions obtained, as well as in the case of a Schwarzschild black hole surrounded by a magnetic field. In all these special situations, the resonant frequencies, Hawking radiation and scattering are studied.     

Development of a new sequential injection in-line cloud point extraction system for flame atomic absorption spectrometric determination of manganese in food samples

A preconcentration method for manganese determination by sequential injection cloud point extraction with subsequent detection by flame atomic absorption spectrometry (FAAS) has been developed. The enrichment of Mn was performed after a preliminary on-line cloud point extraction and entrapment of manganese-containing surfactant aggregated within a minicolumn packed with cotton. The laboratory-made reagent 4-(5′-bromo-2′-thiazolylazo)orcinol (Br-TAO) and the surfactant Triton X-114 were used for cloud point extraction. The manganese ions were eluted with sulphuric acid solution and directly introduced into the FAAS. Chemical and flow variables affecting the preconcentration were studied. Using a sample volume of 2.80 mL the limit of detection and enrichment factor were calculated to be 0.5 μg L⁻¹ and 14, respectively. The sample frequency is 48 h⁻¹, considering a total run cycle of 75 s. The accuracy of the proposed method has been demonstrated by the analysis of the certified reference biological materials rice flour and tomato leaves. The method has been applied to determination of manganese in food samples.     

Identities of *-superalgebras and almost polynomial growth

We study the growth of the codimensions of a *-superalgebra over a field of characteristic zero. We classify the ideals of identities of finite dimensional algebras whose corresponding codimensions are of almost polynomial growth. It turns out that these are the ideals of identities of two algebras with distinct involutions and gradings. Along the way, we also classify the finite dimensional simple *-superalgebras over an algebraically closed field of characteristic zero.     

Influence of the atmosphere on the decomposition of vegetable oils: study of the profiles of FTIR spectra and evolution of gaseous products

Journal of Thermal Analysis and Calorimetry - The thermal stability of vegetable oils may be one of important properties in their use in the food industry, cosmetics and agro-industry, especially...     

Ein Beitrag zum Einfluß des Stoffüberganges auf eine erzwungene Konvektion an einer fluiden Phasengrenze

The interfacial-dynamic behaviour of a fluid two-phase-system with mass transfer was investigated under influence of forced convection in the manner of flat jets directed to the interface. The tangential velocities were measured at a characteristic point near to the interface air/water or in the interface itself using a Laser-Doppler-Velocimeter in dependence on the velocities of jets into two phases in both cases with and without transfer of acetone. The variations of velocities due to the interfacial effects are only detectable at small velocities of the jets. They are discussed by model conceptions and compared with the results of a theoretical research of heat transfer in a fluid two-phase-system (Interfacial-dynamic surface renewal model).     

Effect of Edible Onion (Allium cepa L.) Film on Quality,Sensory Properties and Shelf Life of Beef Burger Patties

The production of edible film from onion (Allium cepa L.) to be applied as packaging is attractive, due to its chemical properties and biodegradable characteristics. Thus, we tested the hypothesis that edible onion film can positively influence the sensory properties, quality and increasing shelf life of beef burgers patties. The experiment was designed in a 4 × 2 factorial scheme, with two treatments (beef burgers patties with or without edible onion film) at an interval of four storage times (0, 3, 6 and 9 days) at 4 °C. The uncoated burger patties (control) suffered the most intense color modifications during the storage (p < 0.05). The luminosity index was higher (p < 0.05) in the control at all storage times, except at day 6, and redness, yellowness and chrome were higher (p < 0.05) in the edible onion film patties at all storage times. The pH of the beef burger patties was lower (p < 0.05) at all storage times when the edible onion film was applied. For the texture profile, only the chewiness was affected, as the inclusion of the edible onion film improved the chewing of the beef burgers patties over the storage time (p < 0.05). Additionally, there was an inhibition of the microbial growth of mesophiles and psychrophiles with the application of the edible onion film in beef burgers patties. The use of edible onion film improved the perception of panelists for the variables texture, color, flavor, odor and overall appearance, and increased the preference of panelists. The edible onion film is recommended for preserving beef burgers patties, as it delays the proliferation of unwanted microorganisms, stabilizes and improves the color parameters and sensory attributes, and increases the overall acceptance of the consumer.     

A column-switching method for quantification of the enantiomers of omeprazole in native matrices of waste and estuarine water samples

This work reports the use of a two-dimensional liquid chromatography (2D-LC) system for quantification of the enantiomers of omeprazole in distinct native aqueous matrices. An octyl restricted-access media bovine serum albumin column (RAM-BSA C₈) was used in the first dimension, while a polysaccharide-based chiral column was used in the second dimension with either ultraviolet (UV-vis) or ion-trap tandem mass spectrometry (IT-MS/MS) detection. An in-line configuration was employed to assess the exclusion capacity of the RAM-BSA columns to humic substances. The excluded macromolecules had a molecular mass in the order of 18 kDa. Good selectivity, extraction efficiency, accuracy, and precision were achieved employing a very small amount (500 μL or 1.00 mL) of native water sample per injection, with detection limits of 5.00 μg L⁻¹, using UV-vis, and 0.0250 μg L⁻¹, using IT-MS/MS. The total analysis time was only 35 min, with no time spent on sample preparation. The methods were successfully applied to analyze a series of waste and estuarine water samples. The enantiomers were detected in an estuarine water sample collected from the Douro River estuary (Portugal) and in an influent sample from the wastewater treatment plant (WWTP) of São Carlos (Brazil). As far as we are concerned, this is the first report of the occurrence of (+)-omeprazole and (−)-omeprazole in native aqueous matrices.     

Performance of anaerobic sequencing batch biofilm reactor submitted to different influent volume feeds and cycle time periods maintaining organic loading

The stability and efficiency of an anaerobic reactor containing biomass immobilized on polyurethane foam were assessed. The reactor with mechanical stirring of 500 rpm and maintained at 30+/-1 degrees C treated synthetic wastewater with a concentration of approx 500 mg of chemical oxygen demand/L and was fed with different influent volumes and cycle times maintaining organic load. Operation was in batch mode with renewal of only part of the volume of wastewater to be treated; that is reactor discharge was not complete, but partial. The main operational characteristic investigated was the ratio of the volume of wastewater fed per cycle (VA) to the volume of wastewater in the reactor (VA) maintaining the same volumetric organic load. This way, operating flexibility could be verified in relation to the volume of treated wastewater at each cycle and the cycle time for the same organic load. The results indicated that the reactor was able to operate with different VA/Vu ratios with no significant loss in performance, thus allowing increased operational flexibility. For conditions in which VA was >or=50% of VA, removal efficiencies of filtered and nonfiltered organic matter were about 84 and 79%, respectively, whereas at conditions of higher initial influent dilution, these efficiencies were slightly lower, about 80 and 74%, respectively. At higher initial influent dilutions, it became difficult to maintain a constant reactor medium volume, owing to a high formation rate of viscous polymer-like material, likely of microbiologic origin.     

Three‐Electrode‐Integrated Sensor into a Micropipette Tip

This work describes the construction, characterization, and application of a three‐electrode‐integrated sensor into a micropipette tip. The three electrodes (working, pseudoreference and counter) are positioned at the end of a micropipette tip. The working electrode (graphite composite or gold microfiber) is placed inside the micropipette tip and the pseudo‐reference and counter electrodes outside (diametrically opposed sides). This approach is candidate for portable applications and allows the analysis and studies in low‐volume solutions (ca. 10 µL) which are useful for waste minimization and development of clean analytical methods. In addition, the three‐electrode‐integrated sensor can be easy used as detector in flow injection system through its direct joining at the end of polyethylene tubing of the FIA system.