10 research outputs found

    Low-Temperature Synthesis and Thermodynamic and Electrical Properties of Barium Titanate Nanorods

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    Studies regarding the morphology dependence of the perovskite-type oxides functional materials properties are of recent interest. With this aim, nanorods (NRs) and nanocubes (NCs) of barium titanate (BaTiO3) have been successfully synthesized via a hydrothermal route at temperature as low as 408 K, employing barium acetate, titanium isopropoxide, and sodium hydroxide as reagents without any surfactant or template. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray powder diffraction (XRD), used for the morphology and structure analyses, showed that the NRs were formed by an oriented attachment of the NCs building-blocks with 20 nm average crystallites size. The thermodynamic properties represented by the relative partial molar free energies, enthalpies, and entropies of the oxygen dissolution in the perovskite phase, as well as the equilibrium partial pressure of oxygen, indicated that NRs powders have lower oxygen vacancies concentration than the NCs. This NRs characteristic, together with higher tetragonallity of the structure, leads to the enhancement of the dielectric properties of BaTiO3 ceramics. The results presented in this work show indubitably the importance of the nanopowders morphology on the material properties

    Electrochemical Sensing of Caffeic Acid Using Gold Nanoparticles Embedded in Poly(3,4-ethylenedioxythiophene) Layer by Sinusoidal Voltage Procedure

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    The increasing demand for sensitive electrochemical sensors in various medical and industrial applications promotes the fabrication of novel sensing materials with improved electrocatalytic and analytical performances. This work deals with the development of a composite material based on gold nanoparticles (AuNPs) embedded in poly(3,4-ethylenedioxythiophene) (PEDOT) layer for electrochemical determination of caffeic acid (CA). CA is a phenolic compound with excellent antioxidant properties that is present in vegetables, fruits, and alcoholic and non-alcoholic beverages. Its analytical quantification is of great interest in food production monitoring and healthcare applications. Therefore, the development of sensitive analytical devices for CA monitoring is required. The AuNPs have been prepared in situ onto PEDOT coated glassy carbon electrode (GC) by means of an innovative procedure consisting on the use of a sinusoidal voltage (SV) superimposed on a constant potential. The physico-chemical properties of the PEDOT-AuNPs composite material were investigated by a range of techniques including cyclic voltammetry, electrochemical quartz crystal microbalance, and scanning electron microscopy. The glassy carbon electrode/poly(3,4-ethylenedioxythiophene)-gold nanoparticles-sinusoidal voltage (GC/PEDOT-AuNPs-SV) sensor exhibited good analytical performance toward the CA quantification with a linear response over a wide concentration range from 10 µM to 1 mM. In addition, the proposed GC/PEDOT-AuNPs-SV sensor was successfully applied in the determination of total polyphenols content expressed as equivalents of CA in juice samples

    Assessment of the Polyphenol Indices and Antioxidant Capacity for Beers and Wines Using a Tyrosinase-Based Biosensor Prepared by Sinusoidal Current Method

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    The application of a novel Poly(3,4-ethylenedioxythiophene)-Tyrosinase/Sonogel-Carbon electrode (PEDOT-Tyr/SNGC) biosensor to beers and wines analysis is proposed. This biosensor implies a new Sinusoidal Current (SC) electrodeposition method to immobilize the enzyme generating a nanostructure surface. The biosensors were characterized electrochemically, employing cyclic voltammetry and electrochemical impedance spectroscopy. Sensitivity, limit of detection, and correlation coefficients of the linear fitting were 2.40 104 A M1, 4.33 M, and R2 = 0.9987, respectively. Caffeic acid is used as the reference polyphenol. A sampling of nine beers (four lager, three stout, and two non-alcoholic beers), and four wines (three red and one white wine) purchased in a local store was performed. The Polyphenol indeces for beers and wines have been assessed using the proposed biosensor, and the obtained values are in agreement with the literature data. Antioxidant properties of the samples using the 2,20-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid (ABTS) radical spectrophotometric method were also evaluated. The correlation between the polyphenol index and the antioxidant capacity was obtained for beers and wines

    Copper(II) Oxide Nanoparticles Embedded within a PEDOT Matrix for Hydrogen Peroxide Electrochemical Sensing

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    The aim of this study is the preparation of nanostructured copper(II) oxide-based materials (CuONPs) through a facile additive-free polyol procedure that consists of the hydrolysis of copper(II) acetate in 1,4-butane diol and its application in hydrogen peroxide sensing. The nonenzymatic electrochemical sensor for hydrogen peroxide determination was constructed by drop casting the CuONP sensing material on top of a glassy carbon electrode (GCE) modified by a layer of poly(3,4-ethylenedioxythiophene) conducting polymer (PEDOT). The PEDOT layer was prepared on GCE using the sinusoidal voltage method. The XRD pattern of the CuONPs reveals the formation of the monoclinic tenorite phase, CuO, with average crystallite sizes of 8.7 nm, while the estimated band gap from UV–vis spectroscopy is of 1.2 eV. The SEM, STEM, and BET analyses show the formation of quasi-prismatic microaggregates of nanoparticles, with dimensions ranging from 1 µm up to ca. 200 µm, with a mesoporous structure. The developed electrochemical sensor exhibited a linear response toward H2O2 in the concentration range from 0.04 to 10 mM, with a low detection limit of 8.5 μM of H2O2. Furthermore, the obtained sensor possessed an excellent anti-interference capability in H2O2 determination in the presence of interfering compounds such as KNO3 and KNO2

    Polyazulene-Based Materials for Heavy Metal Ion Detection. 3. (E)-5-((6-<i>t</i>-Butyl-4,8-dimethylazulen-1-yl) diazenyl)-1H-tetrazole-Based Modified Electrodes

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    A recently synthesized azulene-tetrazole molecular receptor is proposed in this paper to continue the series of azulene substituted compounds that have been developed to build polyazulene-based materials for heavy metal (HM) ion detection. This study focuses on characterization of (E)-5-((6-t-butyl-4,8-dimethylazulen-1-yl) diazenyl)-1H-tetrazole (L) by electrochemical techniques in view of its use for designing electrochemical sensors for HM ion complexation. The character of redox processes was proved by cyclic, differential pulse, and rotating disk electrode voltammetry. An in-depth thermodynamic study of the complexation properties of the free ligand with Pb(II) and Cd(II) from aqueous solutions was performed, and the stoichiometry and stability constant values were determined. Chemically modified electrodes (CMEs) based on L (L-CMEs) prepared by controlled potential electrolysis (CPE) at different applied potentials and charges were characterized by cyclic voltammetry and electrochemical impedance spectroscopy (EIS). Their surface morphology was examined by scanning electron microscopy (SEM). The complexing properties of L-CMEs were investigated towards the detection of HM ions by anodic stripping and compared to the stability constants of the complexes in solution. Voltametric curves showed well-defined peaks for Pb (II), Cd (II), Cu (II) and Hg (II), but the responses differ from each other and vary depending on the ion concentrations in the accumulation solutions. The best results were obtained for Pb(II) and Cd(II) ions. The results obtained for Pb(II) are promising and can be used for its analysis in water solutions (detection limit of about 10−9 M)

    A Sensitive Electrochemical Sensor Based on Sonogel-Carbon Material Enriched with Gold Nanoparticles for Melatonin Determination

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    In this work, the development of an electrochemical sensor for melatonin determination is presented. The sensor was based on Sonogel-Carbon electrode material (SNGCE) and Au nanoparticles (AuNPs). The low-cost and environmentally friendly SNGCE material was prepared by the ultrasound-assisted sonogel method. AuNPs were prepared by a chemical route and narrow size distribution was obtained. The electrochemical characterization of the SNGCE/AuNP sensor was carried out by cyclic voltammetry in the presence of a redox probe. The analytical performance of the SNGCE/AuNP sensor in terms of linear response range, repeatability, selectivity, and limit of detection was investigated. The optimized SNGCE/AuNP sensor displayed a low detection limit of 8.4 nM melatonin in synthetic samples assessed by means of the amperometry technique. The potential use of the proposed sensor in real sample analysis and the anti-matrix capability were assessed by a recovery study of melatonin detection in human peripheral blood serum with good accuracy
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