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1.
Pristine activated carbon (AcC) was oxidized by H2O2 under ultrasonic conditions. Compared with pristine AcC, the H2O2-oxidized AC possesses higher accumulation ability to trace levels of Cd2+. Based on this, a highly sensitive, simple and rapid electrochemical method was developed for the determination of Cd2+. In 0.01 mol L−1 HClO4 solution, Cd2+ was effectively accumulated at the surface of H2O2-oxidized AcC modified paste electrode, and then reduced to Cd under −1.10 V. During the following potential sweep from −1.10 to −0.50 V, reduced Cd was oxidized and a sensitive stripping peak appears at −0.77 V. The stripping peak current of Cd2+ changes linearly with concentration over the range 5.0 × 10−8 to 5.0 × 10−6 mol L−1. The limit of detection was found to be 3.0 × 10−8 mol L−1 for 2-min accumulation. Finally, this new sensing method was successfully used to detect Cd2+ in waste water samples.  相似文献   

2.
Co3O4 nanorods have been successfully synthesized by thermal decomposition of the precursor prepared via a facile and efficient microwave-assisted hydrothermal method, using cetyltrimethylammonium bromide (CTAB) with ordered chain structures as soft template for the first time. The obtained Co3O4 was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and electrochemical measurements. The results demonstrate that the as-synthesized nanorods are single crystalline with an average diameter of about 20 to 50 nm and length up to several micrometers. Preliminary electrochemical studies, including cyclic voltammetry (CV), galvanostatic charge–discharge, and electrochemical impedance spectroscopy (EIS) measurements, are carried out in 6 M KOH electrolyte. Specific capacitance of 456 F g−1 for a single electrode could be achieved even after 500 cycles, suggesting its potential application in electrochemical capacitors. This promising method could provide a universal green chemistry approach to synthesize other low-cost and environmentally friendly transition metal hydroxide or oxide.  相似文献   

3.
In this study, a sensor for the sensitive determination of ascorbic acid (AA) has been fabricated based on meso-tetra-(3,5-dibromo-4-hydroxydroxyphenyl) porphyrin copper (II) (T(DBHP)P-Cu) modified Au electrode through l-cysteine (l-cys). Firstly, l-cys modified Au electrode was prepared through self-assembled technology. Then T(DBHP)P-Cu was adsorbed on l-cys/Au through covalent binding. The fabrication process and electrochemical behavior of T(DBHP)P-Cu/l-cys/Au were studied by cyclic voltammetry and differential pulse voltammetry. The results showed that AA exhibited good electrochemical activity at T(DBHP)P-Cu/l-cys/Au. The oxidation peak current increased linearly with AA concentration in the range of 1.00 × 10−3–1.02 × 10−5 mol L−1 with a detection limit of 5.41 × 10−7 mol L−1. Additionally, the modified electrode could be applied to the detect AA in practical samples.  相似文献   

4.
The xPbTe/Yb0.2Co4Sb12 compounds were prepared by the ball-milling and hot-pressed process. Electrical conductivity of the composite samples are reduced with a increase in PbTe content; and, their temperature dependence coefficients show the positive values. The maximum electrical conductivity of composite materials is ~80000 Sm−1 at 800 K. The Seebeck coefficient (absolute value) of the composite material is obviously improved with an increase in the dispersed phase (PbTe) content; the Seebeck coefficient (absolute value) of the 10PbTe sample is ~260 μVK−1 at 700 K, which increases by 13.6% relative to that of the Yb0.2Co4Sb12 sample. The thermal conductivity of the composite samples is improved due to introduction of PbTe, and the thermal conductivity of the 10PbTe sample is ~3 Wm−1 K−1 at 550 K. The maximum value of ZT is 0.78 at 700 K for the 2.5PbTe sample.  相似文献   

5.
In this study, innovative TiO2/Al2O3 mono/multilayers were applied by atomic layer depositions (ALD) on ASTM-AZ-31 magnesium/aluminum alloy to enhance its well-known scarce corrosion resistance. Four different configurations of ALD layers were tested: single TiO2 layer, single Al2O3 layer, Al2O3/TiO2 bilayer and Al2O3/TiO2/Al2O3/TiO2 multilayer deposited using Al[(CH3)]3 (trimethylaluminum, TMA), and TiCl4 and H2O precursors. All depositions were performed at 120°C to obtain an amorphous-like structure of both oxide layers. The four coatings were then investigated using different techniques, such as scanning electron microscope (SEM), stylus profilometer, glow discharge optical emission spectrometry (GDOES) and polarization curves in 0.05-M NaCl solution. The thickness of all the coatings was around 100 nm. The layers compositions were successfully investigated by the GDOES technique, although obtained data seem to be affected by substrate roughness and differences in sputtering rates between ceramic oxides and metallic magnesium alloy. Corrosion resistance showed to be strongly enhanced by the nanometric coatings, giving lower corrosion current densities in 0.05-M NaCl media with respect to the uncoated substrate (from 10−4 to 10−6 A/cm2 for the single layers and from 10−4 to 10−8 A/cm2 for the bi- and multilayers). All polarization curves on coated samples also showed a passive region, wider for the bi-layer (from −0.58 to −0.43 V with respect to Ag/AgCl) and multilayer (from −0.53 to −0.38 V with respect to Ag/AgCl) structures.  相似文献   

6.
The Sb2O3 doping lead-free glass in Bi2O3-B2O3-BaO ternary system were prepared in the composition of several different subsystem, and the glass powder was produced through the process of water quenching. Glass transition temperatures (T g ), glass soften temperatures(T s ), the volume resistivity (ρ) in the temperature range of 80–200°C, and linear thermal coefficients of expansion in the temperatures range of 25–300°C (α25–300) were measured for subsystems along with the different ratio of Bi2O3, B2O3 and BaO. For these subsystems, T g ranged from 458 to 481°C, and T s ranged from 490 to 512°C, both decreasing with the increasing of Bi2O3/B2O3 ratio, and increasing with the increasing of BaO/B2O3 ratio. The measured α25–300 ranged from 65.3 to 76.3 × 10−7 K−1, with values increasing with increasing Bi2O3/B2O3 and BaO/B2O3 ratio. The volume resistivity remains at a high standards, which may caused by it’s non-alkali composition, and it fluctuated from 1013 to 1011 Ω cm with the temperature varied from 80–200°C. The structure of Bi2O3-B2O3-BaO ternary leadfree glass system was mearsured by FT-IR. The IR studies indicate that these glasses are made up of [BiO6], [BO3], and [BO4] basic structural units, and it appears that Ba2+ acts as a glass-modifier in this ternary system, but the Bi3+ has entered the glass network when it is in relative high content so as to change the α25–300, T s and T g .  相似文献   

7.
Electrooxidation of glutathione (GSH) was studied at the surface of 2,7-bis (ferrocenyl ethyl) fluoren-9-one modified carbon paste electrode (2,7-BFEFMCPE). Cyclic voltammetry (CV), double potential-step chronoamperometry, and differential pulse voltammetry (DPV) were used to investigate the suitability of this ferrocene derivative as a mediator for the electrocatalytic oxidation of GSH in aqueous solutions with various pH. Results showed that pH 7.00 is the most suitable pH for this purpose. At the optimum pH, the oxidation of GSH at the surface of this modified electrode occurs at a potential of about 0.410 V versus Ag|AgCl|KClsat. The kinetic parameters such as electron transfer coefficient, α = 0.61, and rate constant for the chemical reaction between GSH and redox site in 2,7-BFEFMCPE, k h = 1.73 × 103 cm3 mol−1 s−1, were also determined using electrochemical approaches. Also, the apparent diffusion coefficient, D app, for GSH was found to be 5.0 × 10−5 cm2 s−1 in aqueous buffered solution. The electrocatalytic oxidation peak current of GSH showed a linear dependence on the glutathione concentration, and linear calibration curves were obtained in the ranges of 5.2 × 10−5 M to 4.1 × 10−3 M and 9.2 × 10−7 M to 1.1 × 10−5 M with cyclic voltammetry and differential pulse voltammetry methods, respectively. The detection limits (3σ) were determined as 1.4 × 10−5 M and 5.1 × 10−7 M for the CV and DPV methods, respectively. This method was also examined as a selective, simple, and precise new method for voltammetric determination of GSH in real sample such as hemolysed erythrocyte.  相似文献   

8.
High quality crednerite CuMnO2 was prepared by solid state reaction at 950 °C under argon flow. The oxide crystallizes in a monoclinically distorted delafossite structure associated to the static Jahn–Teller (J–T) effect of Mn3+ ion. Thermal analysis showed that it converts reversibly to spinel Cu x Mn3−x O4 at ~420 °C in air and further heating reform the crednerite above 940 °C. CuMnO2 is p-type, narrow semiconductor band gap with a direct optical gap of 1.31 eV. It exhibits a long-term chemical stability in basic medium (KOH 0.5 M), the semi logarithmic plot gave an exchange current density of 0.2 μA cm−2 and a corrosion potential of ~−0.1 VSCE. The electrochemical oxygen insertion/desinsertion is evidenced from the intensity–potential characteristics. The flat band potential (V fb = −0.26 VSCE) and the holes density (N A  = 5.12 × 1018 cm−3) were determined, respectively, by extrapolating the curve C 2 versus the potential to the intersection with C 2  = 0 and from the slope of the Mott–Schottky plot. From photoelectrochemical measurements, the valence band formed from Cu-3d wave function is positioned at 5.24 ± 0.02 eV below vacuum. The Nyquist representation shows straight line in the high frequency range with an angle of 65° ascribed to Warburg impedance originating from oxygen intercalation and compatible with a system under mass transfer control. The electrochemical junction is modeled by an equivalent electrical circuit thanks to the Randles model.  相似文献   

9.
Nickel hydroxide nanosheets were successfully synthesized by facile solvothermal method without any template. The structure and morphology of the as-prepared sample were characterized by X-ray diffraction, Fourier transform infrared spectroscopy and transmission electron microscopy. The observations revealed the formation of hexagonal phase β-Ni(OH)2 nanosheets with an average diameter of about 100–120 nm. Electrochemical studies were carried out using cyclic voltammetry and galvanostatic charge–discharge tests, respectively. A maximum specific capacitance of 2,342 F g−1, which is the highest reported for a β-Ni(OH)2 electrode, could be achieved in 6 mol L−1 KOH electrolyte within the potential range of 0–0.50 V (vs. SCE) for the obtained β-Ni(OH)2 electrode at 0.4 A g−1, suggesting its potential application in the electrode material for electrochemical capacitors.  相似文献   

10.
The Li-rich layered cathode material, Li[Ni0.2Li0.2Mn0.6]O2, was synthesized via a “mixed oxalate” method, and its structural and electrochemical properties were compared with the same material synthesized by the sol–gel method. X-ray diffraction (XRD) shows that the synthesized powders have a layered O3–LiCoO2-type structure with the R-3m symmetry. X-ray photoelectron spectroscopy (XPS) indicates that in the above material, Ni and Mn exist in the oxidation states of +2 and +4, respectively. The layered material exhibits an excellent electrochemical performance. Its discharge capacity increases gradually from the initial value of 228 mA hg−1 to a stable capacity of over 260 mA hg−1 after the 10th cycle. It delivers a larger capacity of 258 mA hg−1 at the 30th cycle. The dQ/dV curves suggest that the increasing capacity results from the redox-reaction of Mn4+/Mn3+.  相似文献   

11.
La0.6Sr0.4Co0.2Fe0.8O3−δ oxides were synthesized by citrate method and hydrothermal method. The oxides prepared by citrate method are perovskite type structure, while the oxides by hydrothermal method have a small amount of secondary phase in the powder. Pyrex glass seal and Ag melting seal provided reliable gas-tight sealing of disk type dense membrane in the range of operation temperature, but commercial ceramic binder could not be removed from the support tube without damage to the tube or membrane. Though the degree of gas tightness increases in the order of glass>Ag>ceramic binder, in the case of glass seal, the undesired spreading of glass leads to an interfacial reaction between it and the membrane and reduction of effective permeation area. The oxygen flux of La0.6Sr0.4Co0.2Fe0.8O3−δ membrane increases with increasing temperature and decreasing thickness, and the oxygen permeation flux through 1.0 mm membrane exposed to flowing air (P h =0.21 atm) and helium (P1=0.037 atm) is ca. 0.33 ml/cm2·min at 950 °C. X-ray diffraction analysis for the membrane after permeation test over 160 h revealed that La2O3 and unknown compound were formed on the surface of membrane. The segregation compounds of surface elements formed on both surfaces of membrane irrespective of spreading of glass sealing material. This paper was presented at the 6 th Korea-China Workshop on Clean Energy Technology held at Busan, Korea, July 4–7, 2006.  相似文献   

12.
The generation of active chlorine on Ti/Sn(1−x)Ir x O2 anodes, with different compositions of Ir (x = 0.01, 0.05, 0.10 and 0.30 ), was investigated by controlled current density electrolysis. Using a low concentration of chloride ions (0.05 mol L−1) and a low current density (5 mA cm−2) it was possible to produce up to 60 mg L−1 of active chlorine on a Ti/Sn0.99Ir0.01O2 anode. The feasibility of the discoloration of a textile acid azo dye, acid red 29 dye (C.I. 16570), was also investigated with in situ electrogenerated active chlorine on Ti/Sn(1−x)Ir x O2 anodes. The best conditions for 100% discoloration and maximum degradation (70% TOC reduction) were found to be: NaCl pH 4, 25 mA cm−2 and 6 h of electrolysis. It is suggested that active chlorine generation and/or powerful oxidants such as chlorine radicals and hydroxyl radicals are responsible for promoting faster dye degradation. Rate constants calculated from color decay versus time reveal a zero order reaction at dye concentrations up to 1.0 × 10−4 mol L−1. Effects of other electrolytes, dye concentration and applied density currents also have been investigated and are discussed.  相似文献   

13.
Titanium (IV) Phosphate copper hexacyanoferrate composite (TiPhCuHCF) was prepared using a new methodology for the synthesis. A preliminary characterization of the precursor and resulting materials was defined using spectroscopic and chemical techniques. The cyclic voltammogram of the modified electrode containing TiPhCuHCF exhibited two redox couples. The first and second redox couples present a formal potential (E θ′) of 0.18 and 0.76 V and were ascribed to the Cu+/Cu2+ (E θ′)1 and Fe2+(CN)6/Fe3+(CN)6 (E θ′)2 processes, respectively. In a preliminary study, the peak located at 0.76 V displays a sensitive response to N-acetylcysteine. The modified graphite paste electrode showed a linear range from 1.0 × 10−5 to 7.0 × 10−4 mol L−1 for the determination of N-acetylcysteine with a limit detection of 6.96 × 10−5 mol L−1 and relative standard deviation of ± 5% (n = 3) and amperometric sensitivity of 24.79 × 10−3 A mol L−1. The modified electrode was electrochemically stable and showed good reproducibility.  相似文献   

14.
The electrocatalytic behavior of uric acid has been investigated with a glassy carbon electrode modified with p-aminobenzene sulfonic acid through electrochemical polymerization. This resulting electrode shows an excellent electrocatalytic response to uric acid and ascorbic acid, with a peak-to-peak separation of 0.267 V in a 0.1 mol L−1 phosphate buffer solution (PBS) at pH 7.0. These results indicate that the proposed electrode can eliminate the serious interference of ascorbic acid, which coexists with uric acid in body fluids. Differential pulse voltammetry (DPV) was used for detecting uric acid with selectivity and sensitivity. The anodic peak current of uric acid was proportional to its concentration in the range of 1.2 × 10−7–8.0 × 10−4 mol L−1, with a detection limit of 4.0 × 10−8 mol L−1. The proposed method has been applied with satisfactory results to the determination of uric acid in human urine without any pretreatment.  相似文献   

15.
Spinel Li4Mn5O12 was prepared by a sol–gel method. The manganese oxide and activated carbon composite (MnO2-AC) were prepared by a method in which KMnO4 was reduced by activated carbon (AC). The products were characterized by XRD and FTIR. The hybrid supercapacitor was fabricated with Li4Mn5O12 and MnO2-AC, which were used as materials of the two electrodes. The pseudocapacitance performance of the Li4Mn5O12/MnO2-AC hybrid supercapacitor was studied in various aqueous electrolytes. Electrochemical properties of the Li4Mn5O12/MnO2-AC hybrid supercapacitor were studied by using cyclic voltammetry, electrochemical impedance measurement, and galvanostatic charge/discharge tests. The results show that the hybrid supercapacitor has electrochemical capacitance performance. The charge/discharge test showed that the specific capacitance of 51.3 F g−1 was obtained within potential range of 0–1.3 V at a charge/discharge current density of 100 mA g−1 in 1 mol L−1 Li2SO4 solution. The charge/discharge mechanism of Li4Mn5O12 and MnO2-AC was discussed.  相似文献   

16.
A series of nano-granular films composed of magnetic metal (Fe65Co35) granules with a few nanometers in size and semiconductor oxide (ZnO) have been fabricated by a magnetron sputtering method, and excellent soft magnetic properties have been achieved in a wide metal volume fraction (x) range for as-deposited samples due to the exchange coupling between FeCo granules (a ferromagnetic interaction in nano-scale). In a wide range (0.53 < x < 0.71), the films exhibit coercivity H C not exceeding 15 Oe, along with high resistivity. Especially for the sample with x = 0.67, coercivities in hard and easy axes are 1.43 and 7.08 Oe, respectively, 4πM S  = 9.85 kg, and ρ reaches 2.06 × 103 μΩ cm. The dependence of complex permeability μ = μ′ − ″ on frequency shows that the real part μ′ is more than 100 below 1.83 GHz and that the ferromagnetic resonance frequency reaches 2.31 GHz, implying the promising for high frequency application. The measured negative temperature coefficient of resistivity reveals that may be the weak localized electrons existing in samples mediate the exchange coupling.  相似文献   

17.
LiMn2O4/multi-walled carbon nanotubes (MWNTs) composite was synthesized by mechanical activation reaction followed by a heat-treatment (500 °C). The LiMn2O4 and LiMn2O4/MWNTs as cathodes were investigated in 1 M Li2SO4 by cyclic voltammetry (CV), galvanostatic charge/discharge (GC), and electrochemical impedance spectroscopy (EIS). The LiMn2O4/MWNTs cathode delivered higher discharge capacity (117 mAh g−1) than LiMn2O4 (84.6 mAh g−1). Furthermore, the results from EIS showed that LiMn2O4/MWNTs had a faster kinetic process for lithium ion intercalation/de-intercalation than LiMn2O4. Besides, LiMn2O4/MWNTs had better cycling stability and rate capability than LiMn2O4, which was confirmed by GC testing. SEM images showed that a three-dimensional network structure was formed during the mechanical activation, giving a decrease of particle size.  相似文献   

18.
A novel DNA electrochemical biosensor is described for the detection of neomycin phosphotransferase gene (NPT-II), a selection marker for transgenic plants. A thiol-modified capture probe immobilized onto the surface of a gold electrode and a biotinylated signaling probe were designed to be complementary to target regions of NPT-II flanked by PCR primers to eliminate false-positive signals from non-specific PCR products. The electrochemical assay of hybrids on the electrode surface was evaluated by means of both cyclic voltammetry (CV) and square wave voltammetry (SWV) after the coupling of biotinylated catalase with streptavidin-modified hybrids based on dendritic signal magnification and subsequent formation of polymerized aniline (PAn). It has been revealed that the sensor showed a linear increase within the target concentration (1.0–100 × 10−6 mmol L−1). The limit of detection was about 0.2 × 10−6 mmol L−1 and the specificity was enhanced significantly.  相似文献   

19.
A Th4+ ion-selective membrane sensor was fabricated from poly (vinyl chloride) (PVC) matrix membrane containing 2-(diphenylphosphorothioyl)-N′,N′-diphenyl acetamide (DPTD) as a neutral carrier, potassium tetrakis (p-chlorophenyl) borate (KTpClPB) as anionic excluder and o-nitrophenyloctyl ether (NPOE) as a plasticizing solvent mediator. The effects of the membrane composition, pH and additive anionic influence on the response properties were investigated. The sensor, comprising 30% PVC, 63% solvent mediator, 4% ionophore and 3% anionic additive demonstrates the best potentiometric response characteristics. It displays Nernstian behavior (15.2 ± 0.5 mV per decade) over the concentration range 1.0 × 10−2–1.0 × 10−6 M. The detection limit of the electrode is 6.3 × 10−7 M (∼140 ng/ml). The response time of the electrode is 30 s .The sensor can be used in the pH range 3.0–9.0 for about 6 weeks. The membrane sensor was used as an indicator electrode in the potentiometric titration of Th4+ ions with EDTA. It was successfully applied to the determination of thorium ions in binary mixture.  相似文献   

20.
The effect of surface area on the electrochemical properties and thermal stability of Li[Ni0.2Li0.2Mn0.6]O2 powders was characterized using a charge/discharge cycler and DSC (Differential Scanning Calorimeter). The surface area of the samples was successfully controlled from ~4.0 to ~11.7 m2 g−1 by changing the molar ratio of the nitrate/acetate sources and adding an organic solvent such as acetic acid or glucose. The discharge capacity and rate capability was almost linearly increased with increase in surface area of the sample powder. A sample with a large surface area of 9.6–11.7 m2 g−1 delivered a high discharge capacity of ~250 mAh g−1 at a 0.2 C rate and maintained 62–63% of its capacity at a 6 C rate versus a 0.2 C rate. According to the DSC analysis, heat generation by thermal reaction between the charged electrode and electrolyte was not critically dependent on the surface area. Instead, it was closely related to the type of organic solvent employed in the fabrication process of the powder.  相似文献   

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