Modified carbon paste electrodes for Cu(II) determination

A new Cu²⁺ carbon paste electrode (CPE) using 2,2′-(1E,1′E)-1,1′-(2,2′-azanediylbis (ethane-2,1-diyl)bis(azan-1-yl-1-ylidene))bis(ethan-1-yl-1-ylidene)diphenol (ADEZEDP) has been prepared. The influence of variables including sodium tetraphenylborate (NaTPB), ionophore, and amount of multiwalled carbon nanotubes (MWCNT), CdO nanowires, CdS nanoparticles and palladium nanoparticles loaded on ADEZEDP and Nujol on the electrodes response were studied and optimized. At optimum values of all variables, for each nanomaterial the electrode response was linear in concentration range of 1.0 × 10^? 8 to 1.0 × 10^? 1 mol L^? 1 for ADEZEDP with Nernstian slope. The good performance of electrode viz. Wide applicable pH range (2.0–5.0), fast response time (≈ 6 s), and adequate life time (3 months) indicate the utility of the proposed electrodes for evaluation of Cu²⁺ ion content in various situations. Finally, these electrodes have been successfully applied for the determination of Cu²⁺ ions content in various real samples. The selectivity of proposed electrode was evaluated by separation solution method and fixed interference method.     

Electrochemical detection of arsenic(III) using iridium-implanted boron-doped diamond electrodes

Iridium-modified, boron-doped diamond electrodes fabricated by an ion implantation method have been developed for electrochemical detection of arsenite (As(III)). Ir+ ions were implanted with an energy of 800 keV and a dose of 10(15) ion cm(-2). An annealing treatment at 850 degrees C for 45 min in H2 plasma (80 Torr) was required to rearrange metastable diamond produced by an implantation process. Characterization was investigated by SEM, AFM, Raman, and X-ray photoelectron spectroscopy. Cyclic voltammetry and flow injection analysis with amperometric detection were used to study the electrochemical reaction. The electrodes exhibited high catalytic activity toward As(III) oxidation with the detection limit (S/N = 3), sensitivity, and linearity of 20 nM (1.5 ppb), 93 nA microM(-1) cm(-2), and 0.999, respectively. The precision for 10 replicate determinations of 50 microM As(III) was 4.56% relative standard deviation. The advantageous properties of the electrodes were its inherent stability with a very low background current. The electrode was applicable for analysis of spiked arsenic in tap water containing a significant amount of various ion elements. The results indicate that the metal-implanted method could be promising for controlling the electrochemical properties of diamond electrodes.     

碳纳米管的电化学性质及其应用研究

把碳纳米管作为一种新型的电极材料是开发碳纳米管应用的一个新的方向。本文研究了碳纳米管的化学修饰和电化学性质,发现决定碳纳米管电化学性质的两个重要因素。系统地总结了我们在碳纳米管电极的制备、碳纳米管电极的电化学响应、碳纳米管电极的生物电分析和电氧化有毒化成分应用方面的研究成果。     

Green synthesis of silver nanoparticles and their applications as colorimetric probe for determination of Fe3+ and Hg2+ ions

Silver nanoparticles (AgNPs) were prepared by a green method using Cordia myxa leaf extract. They were characterised by UV–vis spectroscopy, Fourier transform infrared spectroscopy and their X‐ray diffraction pattern. Their sizes were determined by scanning electron micrographs, transmission electron micrographs imaging and dynamic light scattering analysis. The shapes of nanoparticles were spherical or truncated triangular and their average size was determined to be 51.6 nm. Their solution was stable at least for one month. The prepared AgNPs were used as a selective chemical sensor for determination of iron(III) (only when Cl⁻ ions were present in the medium) and mercury(II) ions with detection limits of 0.084 and 0.037 nM, respectively. It was shown that the mechanism of these detections is through oxidation of Ag atoms by Fe³⁺ and Hg²⁺ ions.Inspec keywords: visible spectra, nanoparticles, transmission electron microscopy, nanofabrication, ultraviolet spectra, chemical sensors, scanning electron microscopy, silver, X‐ray diffraction, Fourier transform infrared spectra, oxidationOther keywords: Ag, Cordia myxa leaf extract, iron(III) ions, mercury(II) ions, oxidation, scanning electron micrographs, Fourier transform infrared spectroscopy, silver nanoparticles, chemical sensor, dynamic light scattering analysis, transmission electron micrographs, X‐ray diffraction pattern, UV–vis spectroscopy, colorimetric probe, green synthesis     

Electrochemical behaviour of graphene–poly (3,4-ethylenedioxythiophene) (PEDOT) composite electrodes for supercapacitor applications

In this paper, we report on the electrochemical characteristics of graphene–PEDOT composite electrodes. The electrodes were made of indium tin oxide (ITO) substrates by simple processes of electrophoretic deposition of graphene followed by electropolymerization of EDOT monomer. The composite electrode was obtained by electrochemical measurements, a median specific capacitance of 1410 F/g and a median area capacitance of 199 mF cm ^?2 at a scan rate of 40 mVs ^?1. The composite showed good stability characteristics after repeated scans in cyclic voltammmetry and fared much better than a thin film of PEDOT. The thermal stability of the composite is also much superior when compared to the polymer with a weight loss temperature of 350 °C for the composite and 250 °C for the polymer, respectively. The above electrochemical and thermal behaviours of the composite are correlated to the unique morphology of electrodeposited graphene that provides a conductive and high surface area template for electropolymerization.     

Membrane optode for mercury(II) determination in aqueous samples

A color changeable optode for Hg(II) was prepared by the immobilization of a dye 4-(2-pyridylazo)resorcinol (PAR) and a liquid ion-exchanger trioctylmethylammonium chloride (Aliquat-336) in the tri-(2-ethylhexyl) phosphate plasticized cellulose triacetate matrix. Hg(II) and CH₃Hg⁺ from aqueous samples could be quantitatively preconcentrated in this transparent optode producing a distinct color change (λ_max = 520 nm) within 5 min equilibration time in bicarbonate aqueous medium or 30 min in natural water. Whereas optode sample without Aliquat-336 did not change its color corresponding to Hg–PAR complex on equilibrium with the same aqueous solution containing Hg(II) ions. The uptake of Hg(II) was found to be pH dependant with a maximum (>90%) at a pH 7.5. The uptake of ions like Cu(II), Fe(II), Zn(II) and Pb(II) was negligible in the optode where as the uptake of Cd(II) and Zn(II) ions was 10–15% at pH 7.5. The optode developed in the present work was studied for its analytical application for Hg(II) in the aqueous samples by spectrophotometry, radiotracer (²⁰³Hg), Energy Dispersive X-ray Fluorescence (EDXRF) analyses and Instrumental Neutron Activation Analysis (INAA). The minimum amount of Hg(II) required to produce detectable response by spectrophotometry, INAA and EDXRF were found to be 5.5, 1 and 12 μg, respectively. This optode showed a linear increase in the absorbance at λ_max = 520 nm over a concentration range of 0.22–1.32 μg/mL of Hg(II) ions in aqueous solution for 5 min. The preconcentration of Hg(II) from large volume of aqueous solution was used to extend the lower limit of concentration range that can be quantified by the spectrophotometry of optode. It was observed that preconcentration of 11 μg Hg(II) in 100 mL (0.11 μg/mL) in aqueous samples gives a distinct color change and absorbance above 3σ of the blank absorbance. The optode developed in the present work was found to be reusable.     

Preparation of metal-polymer composites through the thermolysis of Fe(II), Co(II), and Ni(II) maleates

Metal-polymer composites have been prepared through the thermolysis of the [M₁(H₂O)₂(C₄H₂O₄)] · H₂O (M₁ = Co(II), Ni(II)) neutral maleates and [M₂(H₂O)₄(C₄H₃O₄)₂] (M₂ = Fe(II), Co(II), Ni(II)) acid maleates. In the polymer matrix of the Fe-containing composite, we identified metal, Fe₂O₃, and Fe₃O₄ particles, with slight densification of the matrix around them. The polymer matrix of the cobalt maleate-derived composite contained four types of nanoparticles: α-Co, β-Co, and CoO in polymer shells and Co₃O₄ with no polymer shell. The decomposition of the nickel maleates yielded homogeneous nickel nanoparticles (4–5 nm) covered with two to five graphene layers. The Co-containing composite was found to be a dielectric. The Ni-containing composite exhibited variable range hopping conduction in the range T ≤ 50 K.     

A comparative study for the ion exchange of Fe(III) and Zn(II) on zeolite NaY

The uptake capacity of Fe(III) and Zn(II) ions in NaY zeolite was investigated. Experiments were carried out in a fixed bed column at 30 degrees C, pH 3.5 and 4.5 for Fe(III) and Zn(II), respectively, and an average particle size of 0.180 mm. In order to minimize the diffusional resistances the influence of flow rate on the breakthrough curves at feed concentrations of 1.56 meq/L for Fe(III) and 0.844 meq/L for Zn(II) was investigated. Flow rate of the minimal resistance in the bed according to mass transfer parameter were 2.0 mL/min for iron and 8.0 mL/min for zinc ions. Freundlich and Langmuir isotherm models have been used to represent the column equilibrium data. The iron dynamic isotherm was successfully modeled by the Langmuir equation and this mathematical model described well the experimental breakthrough curves for feed concentrations from 0.1 up to 3.5 meq/L. The zinc dynamic isotherm was successfully modeled by the Freundlich equation. This equilibrium model was applied to mathematical model. Experimental breakthrough curves could be predicted. Experiments were also carried out in a batch reactor to investigate the kinetics adsorption of the ions Fe(III) and Zn(II). Langmuir kinetic model fit well both experimental data.     

Magnetic nanobiosorbent (MG‐Chi/Fe3O4) for dispersive solid‐phase extraction of Cu(II), Pb(II), and Cd(II) followed by flame atomic absorption spectrometry determination

Trace amounts of Cu (II), Pb (II), and Cd (II) in a wastewater sample were preconcentrated with a novel cross‐linked magnetic chitosan modified with a new synthesised methionine‐glutaraldehyde Schiff''s base (MG‐Chi/Fe₃O₄) as a dispersive solid‐phase extraction (DSPE) adsorbent. The adsorbed metal ions were then eluted with a specific volume of suitable solution and determined by flame atomic absorption spectrometry (FAAS). Various parameters affecting the extraction efficiency of the metal ions were investigated and optimised, including pH, amount of adsorbent, extraction time, type and volume rate of eluent, elution time, sample volume, and effect of interfering ions. The adsorption kinetics are more consistent with the pseudo‐second order model. The results were statistically interpreted and the analytical performance of the proposed method was found to have preconcentration factors of 55, 60, and 50 μg L⁻¹ for Cu(II), Pb(II), and Cd(II), respectively, limits of detection were 0.22, 0.24, and 0.10 μg L⁻¹ for Cu(II), Pb(II), and Cd(II), respectively, with a relative standard deviation (1.5%‐2.8 %), and the liner range was 5–1000 for Cu(II) and Pb(II) and 2.5–1000 for Cd(II). It was concluded that this method was suitable for successful simultaneous determination of Cu(II), Pb(II), and Cd(II) in industrial wastewater samples.     

High temperature (Tc) superconductors and their possible applications

The background of the recent discovery of high temperature oxide superconductors is given. The new class of materials poses many challenges to researchers and raises many exciting possibilities in technological and industrial applications. To physicists and chemists there are the questions of why this particular structure and type of compounds and what is the mechanism for superconductivity; to material scientists and electronic engineers there remain many questions concerning the preparation and the stability of the materials in forms suitable for thin film as well as heavy current uses.     

Sorption-catalytic method for the determination of copper (II) in combination with planar chromatography

An activating action of hexamethylenediamine is revealed in the copper (II)-catalyzed indicator reaction of iron (III) reduced by sodium thiosulfate. It is shown that the addition of hexamethylenediamine to a mobile phase (thin-layer chromatography) and the impregnation of paper with hexamethylenediamine (paper chromatography) enhance the efficiency of metal separation for the model mixture containing Cu (II), Hg (II), Cd (II), and Pb (II). The techniques for the sorption-catalytic determination of copper (II) with the help of Sorbfil plates, including those in combination with thin-layer chromatography, are developed; they work within the concentration range from 0.005 to 10 ??g/mL, the detection limit being 4 ng/mL, which is approximately an order of magnitude lower than in solution. The methods are tested in analysis of waste and river waters.     

Synthesis and characterization of Cu(II) containing PMMA co-polymer for optical applications

Homogenous, transparent, greenish blue Cu(II) containing PMMA co-polymer disks were prepared through the radical polymerization of the Cu(II) methacrylate, MMA and HMA using AIBN as an initiator. The dependence of the absorbance and transmittance spectra with the Cu(II) methacrylate concentration was investigated in the visible range (420–750 nm). From the transmittance measurements the refractive index and extinction coefficient spectral dependence were calculated by application of an inversion approach. To further characterize this co-polymer a thermogram was performed. The overall behavior of this material suggests its possible use as a standard solution for Spectroscopy Equipment Calibration and as a selective optical filter.     

Coprecipitation of gold(III), palladium(II) and lead(II) for their flame atomic absorption spectrometric determinations

An enrichment-separation procedure based on the coprecipitation of gold(III), palladium(II) and lead(II) ions with nickel(II)-5-methyl-4-(2-thiazolylazo) resorcinol complex has been developed. The analytical parameters including pH, amounts of 5-methyl-4-(2-thiazolylazo) resorcinol, sample volume, etc. was investigated for quantitative recoveries of Au(III), Pd(II) and Pb(II). Interference due to various cations and anions has also been investigated. The detection limits for analyte ions by 3sigma were 2.6 microg L(-1) for lead, 1.5 microg L(-1) for gold, 2.1 microg L(-1) for palladium. The accuracy of the method was evaluated by the analysis of certified reference materials (NIST SRM 2711 Montana soil, GBW 07309 Stream sediment). The proposed procedure was successfully applied to environmental samples for the determinations of analytes.     

Dye-sensitized nickel(II)oxide photocathodes for tandem solar cell applications

To date, nickel(II) oxide (NiO) is one of the few p-type semiconductors that has successfully been used for the construction of dye-sensitized photocathodes as well as tandem dye-sensitized solar cells. In this study we present a novel fabrication method for the preparation of mesoporous NiO films based on preformed NiO nanopowders. Critical properties such as pore-size distribution, crystallinity, and internal surface area of the resulting NiO films were controlled through the sintering process and optimized for their application as dye-sensitized photocathodes, resulting in a significantly increased photovoltaic performance, compared to earlier studies. A series of different sensitizers and electrolytes was scrutinized for their application in dye-sensitized NiO photocathodes. Despite its limited absorption range the dye coumarin 343 clearly outperforms other sensitizers used in this study. Values for short-circuit current densities of 2.13?mA?cm(-2) and overall energy conversion efficiencies of 0.033% under simulated sunlight (AM1.5, 1000?W?m(-2)) are the highest values reported in literature so far.     

Preparation and XPS studies of macromolecule mixed-valent Cu(I, II) and Fe(II, III) complexes

A new macromolecule ligand and its mixed-valent Cu(I, II) and Fe(II, III) complexes have been prepared by using ethylenediamine as core and maleic anhydride as branched units and characterized by UV-vis, FT-IR, thermal analysis and X-ray photoelectron spectroscopy (XPS). The data obtained from these studies suggested that the coordinate bonds of N-->M, Cl-->M, Ph-OH-->M and H(2)O-->M have been formed and possible binding models are proposed for these complexes. The thermal analysis (TG-DTG) reveals that these complexes possess thermal stable property below 800 degrees C.     

Lead (II) ion selective electrodes based ondiphenylmethyl-N-phenylhydroxamic acid ionophore in cyanocopolymermatrix

A Pb²⁺ ion selective electrode has been prepared using diphenylmethyl-N-phenylhydroxamic acid (DPNINPRA) as ionophore and cyanocopolymer as new membrane matrix. The electrode (Membrane-2) exhibited a Nernstian slope of 36.75±0.001 mV decade^-1 activity of Pb²⁺ ions on varying the Pb²⁺ ions activity from 7.41×10^-8 to 3.68×10^-1 mol dm^-3. The electrode has exhibited a response time of 13.0±s at 1.0×10^-3 mol dm^-3 activity of Pb²⁺ ions and also revealed an improved selectivity in presence of various interfering ions. The high dipolar property of the selected cyanocopolymer has reduced significantly the anions interference and shown potential response independent to the activity of sodium tetraphenylborate (NaTPB). The electrode has shown isothermal point of 30°C as determined from a hysteresis curve. Sensitivity of the electrode has shown a significant variation with thickness of the membrane. The electrode has shown a constant response on continuous use for a period of six months without any drift in potential and has been also found to be useful as indicator electrode for potentiometric titration of Pb²⁺ ions