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A highly sensitive analytical method was developed to determine 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and 2,3,4,5,6-pentachloroanisole (PCA) in sparkling alcoholic beverages. The method was based on the use of headspace solid-phase microextraction (HS-SPME) using a polydimethylsiloxane (PDMS) fibre. It was coupled to gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS/MS) for the detection and quantification of the target haloanisoles. The method was fully automated and no sample preparation was needed. The method was validated for alcoholic beverages. The influence of CO2on the extraction efficiency was also evaluated for the studied sparkling drinks (cava and cider). All the calibration curves showed good linearity (R2 > 0.98) within the tested range (1–50 ng l−1). Recoveries were evaluated at three different levels (1, 5 and 50 ng l−1) and were always between 71% and 119%. Precision was expressed as relative standard deviation (RSD), and was evaluated as intra- and inter-day precisions, with values ≤ 22% in both cases. Limits of quantitation (LOQs) were ≤ 0.91 ng l−1, which are below the sensory threshold levels for such compounds in humans. The validated method was applied to commercial samples, 10 cavas and 10 ciders, but it was also used for the analysis of nine red wines and four white wines, demonstrating the further applicability of the proposed method to non-sparkling beverages. TCA was detected in most samples at up to 0.45 ng l−1. [ABSTRACT FROM PUBLISHER]

Thirteen polycyclic aromatic hydrocarbons have been determined in soy-based nutraceutical products. First, an optimization of extraction procedure was performed, and a solid-liquid extraction assisted by sonication and a dilute and shoot procedure were compared, selecting the dilute and shoot approach for the extraction of target compounds, utilizing a mixture of acetone/ n-hexane (1:1 v/v) as extractant solvent. After this, a clean-up step was needed bearing in mind the complexity of these matrices. Dispersive solid-phase extraction, using a mixture of C18 and Zr-Sep+ (25 mg/mL each) was used. The separation was achieved by gas chromatography and detection with triple quadrupole tandem mass spectrometry. For quantification purposes, matrix-matched calibration was used. The validation was applied at three concentration levels (20, 100 and 250 μg/kg), obtaining recoveries between 70 and 120% and precision values equal to or lower than 23%. Limits of detection and quantification were below 8 and 20 μg/kg, respectively. The method was applied in 11 samples, detecting five polycyclic aromatic hydrocarbons at concentrations ranging from 4.1 to 18.5 μg/kg. [ABSTRACT FROM AUTHOR]

Several beneficial features maintain TiO 2 in the top list of viable materials for photocatalytic purposes. However, its relatively large band-gap (3.0–3.2 eV) still hampers practical applications under sunlight. This work explores Direct Current (DC) Plasma Electrolytic Oxidation (PEO) of titanium as a fast, easily-scalable and single-step tool to synthesise doped TiO 2 photoanodes with controlled morphology, crystalline structure and thickness. Zn-, Cu- and Fe-doped crystalline TiO 2 films were obtained in H 2 SO 4 aqueous solutions containing ZnSO 4 , CuSO 4 and FeSO 4 precursors, respectively. As-prepared TiO 2 films showed a porous and homogeneous sponge-like surface morphology, typical of PEO-produced oxides, and a crystalline phase structure consisting of a mixture of anatase and rutile phases. The anatase content varied in the 54–100 % range and correspondingly the band-gap energy was in the 2.85–3.07 eV range. Doped oxides prepared with a low concentration of the metal precursors showed monochromatic incident-photon-to-current-efficiency (IPCE) values exceeding those obtained with pristine TiO 2 by up to 24 %, best performing in the order Zn- > Cu- > Fe-doped TiO 2. Photocurrent under polychromatic UV-Vis irradiation showed an analogous trend and the estimated efficiency of solar-light harvesting was in the 0.3–4 % range, with Zn- ≈ Cu- > Fe-doped TiO 2. Although the superior performance of the PEO-prepared metal-doped TiO 2 could not be fully confirmed by photoelectrocatalytic oxidation tests of organics, the present investigation showed the viability of DC PEO for the synthesis of metal-doped TiO 2 photoanodes. [Display omitted] • Zn, Cu, Fe doped crystalline TiO 2 films obtained by plasma electrolytic oxidation. • Best photoeletrochemical activity at low doping levels. • IPCE and LSV values exceeding pristine TiO 2. • No straightforward correlation between photoelectrochemical and catalytic activity. [ABSTRACT FROM AUTHOR]

The development of treatment trains for pollutant degradation employing zerovalent iron has been attracting a lot of interest in the last few years. This approach consists of pre-treatment only with zerovalent iron, followed by a Fenton oxidation taking advantage of the iron ions released in the first step. In this work, the advantages/disadvantages of this strategy were studied employing commercial zerovalent iron microparticles (mZVI). The effect of the initial amount of mZVI, H2O2, pH, conductivity, anions and dissolved oxygen were analysed using p-nitrobenzoic acid (PNBA) as model pollutant. 83% reduction of PNBA 6 µM into p-aminobenzoic acid (PABA) was achieved in natural water at an initial pH 3.0 and 1.4 g/L of mZVI, under aerobic conditions, in 2 h. An evaluation of the convenience of removing mZVI after the reductive phase before the Fenton oxidation was investigated together with mZVI reusability. The Fenton step against the more reactive PABA required 50 mg/L of H2O2 to achieve more than 96% removal in 15 min at pH 7.5 (final pH from the reductive step). At least one complete reuse cycle (reduction/oxidation) was achieved with the separated mZVI. This approach might be interesting to treat wastewater containing pollutants initially resistant to hydroxyl radicals. [ABSTRACT FROM AUTHOR]