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1.
A simple procedure has been used for preparation of modified glassy carbon electrode with carbon nanotubes and copper complex. Copper complex [Cu(bpy)2]Br2 was immobilized onto glassy carbon (GC) electrode modified with silicomolybdate, α-SiMo12O404− and single walled carbon nanotubes (SWCNTs). Copper complex and silicomolybdate irreversibly and strongly adsorbed onto GC electrode modified with CNTs. Electrostatic interactions between polyoxometalates (POMs) anions and Cu-complex, cations mentioned as an effective method for fabrication of three-dimensional structures. The modified electrode shows three reversible redox couples for polyoxometalate and one redox couple for Cu-complex at wide range of pH values. The electrochemical behavior, stability and electron transfer kinetics of the adsorbed redox couples were investigated using cyclic voltammetry. Due to electrostatic interaction, copper complex immobilized onto GC/CNTs/α-SiMo12O404− electrode shows more stable voltammetric response compared to GC/CNTs/Cu-complex modified electrode. In comparison to GC/CNTs/Cu-complex the GC/CNTs/α-SiMo12O404− modified electrodes shows excellent electrocatalytic activity toward reduction H2O2 and BrO3 at more reduced overpotential. The catalytic rate constants for catalytic reduction hydrogen peroxide and bromate were 4.5(±0.2) × 103 M−1 s−1 and 3.0(±0.10) × 103 M−1 s−1, respectively. The hydrodynamic amperommetry technique at 0.08 V was used for detection of nanomolar concentration of hydrogen peroxide and bromate. Detection limit, sensitivity and linear concentration range proposed sensor for bromate and hydrogen peroxide detection were 1.1 nM and 6.7 nA nM−1, 10 nM-20 μM, 1 nM, 5.5 nA nM−1 and 10 nM-18 μM, respectively.  相似文献   

2.
Pt nanoclusters were deposited in polypyrrole (PPy) nanowires by cyclic voltammetry method, fabricating a PPy-Pt nanocomposite on glassy carbon electrode (PPy-Pt/GCE). The electrocatalytic reduction of nitrite at PPy-Pt/GCE has been investigated using 0.5 M H2SO4 solution. The sensor exhibited excellent electrocatalytic activity toward nitrite reduction. In acidic medium, the cyclic voltammetry at 20 mV s− 1 gave a nitrite reduction peak at − 0.124 V with 0.566 μA μM− 1 current sensitivity in the range of 5.0 × 10− 7-1.0 × 10− 3 M. The detection limit was 1.5 × 10− 7 M (s/n = 3). The proposed method was successfully applied in the detection of nitrite in real water samples and obtained satisfactory results. The PPy-Pt composite modified electrode had good storage stability, reproducibility and anti-interference ability.  相似文献   

3.
A new palladium nanoparticle functionalized multi-wall carbon nanotubes (nano-Pd/CNTs) modified pyrolytic graphite electrode (PGE) has been fabricated for electrochemical sensing of calcium dobesilate (CD) in pharmaceutical capsules. The nano-Pd/CNTs were characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The nano-Pd/CNTs composite showed a strong electrocatalytic property for CD. The anodic peak current is 6-fold than that obtained in bare PGE and the oxidation potential has an obvious shift to negative. The anodic peak current is proportional to the concentration of CD in the range of 1.0 × 10−7 to 7.0 × 10−4 mol L−1, with a linear relative coefficient r = 0.999 and a detection limit 4.0 × 10−8 mol L−1 (S/N = 3). This kind of electrode shows good stability, sensitivity, reproducibility, large linear range and low detection limit towards electrochemical determination of CD. The proposed method provides a selective and sensitive electrochemical sensor of calcium dobesilate.  相似文献   

4.
An electrochemiluminescence (ECL) sensor based on Ru(bpy)32+-graphene-Nafion composite film was developed. The graphene sheet was produced by chemical conversion of graphite, and was characterized by atomic force microscopy (AFM), scanning electron microscopy (SEM), and Raman spectroscopy. The introduction of conductive graphene into Nafion not only greatly facilitates the electron transfer of Ru(bpy)32+, but also dramatically improves the long-term stability of the sensor by inhibiting the migration of Ru(bpy)32+ into the electrochemically inactive hydrophobic region of Nafion. The ECL sensor gives a good linear range over 1 × 10−7 to 1 × 10−4 M with a detection limit of 50 nM towards the determination of tripropylamine (TPA), comparable to that obtained by Nafion-CNT. The ECL sensor keeps over 80% and 85% activity towards 0.1 mM TPA after being stored in air and in 0.1 M pH 7.5 phosphate buffer solution (PBS) for a month, respectively. The long-term stability of the modified electrode is better than electrodes modified with Nafion, Nafion-silica, Nafion-titania, or sol-gel films containing Ru(bpy)32+. Furthermore, the ECL sensor was successfully applied to the selective and sensitive determination of oxalate in urine samples.  相似文献   

5.
A polyaniline (PANI)/carbon nanotubes (CNTs) composite modified electrode was fabricated by galvanostatic electropolymerization of aniline on multi-walled carbon nanotubes (MWNTs)-modified gold electrode. The electrode thus prepared exhibits enhanced electrocatalytic behavior to the reduction of nitrite and facilitates the detection of nitrite at an applied potential of 0.0 V. Although the amperometric responses toward nitrite at MWNTs/gold and PANI/gold electrodes have also been observed in the experiments, these responses are far less than that obtained at PANI/MWNTs/gold electrode. The effects of electropolymerization time, MWNTs concentration and pH value of the detection solution on the current response of the composite modified electrode toward sodium nitrite, were investigated and discussed. A linear range from 5.0 × 10−6 to 1.5 × 10−2 M for the detection of sodium nitrite has been observed at the PANI/MWNTs modified electrode with a sensitivity of 719.2 mA M−1 cm−2 and a detection limit of 1.0 μM based on a signal-to-noise ratio of 3.  相似文献   

6.
Wen ZH  Kang TF 《Talanta》2004,62(2):351-355
An amperometric nitrite sensor based on a polymeric nikel tetraaminothphalocyanine (p-NiTAPc) film coated glassy carbon (GC) electrode was developed. The mechanism of catalysis on the surface of the electrode was discussed. The sensor exhibited fast respond towards nitrite with a detection limit of 1×10−7 M and a linear concentration range of 5×10−7 to 8×10−3 M. The possible interference from several common ions was tested. The proposed method was successfully applied in the detection of nitrite in real samples.  相似文献   

7.
Titanium oxide/carbon nanotubes-based nanocomposites (TiO2/CNTs, prepared by sol-gel method, and 2%Pt/TiO2/CNTs, obtained by wetness impregnation of the TiO2/CNTs base material with a solution of platinum acetylacetonate) have been recently used as active layer in hydrogen sensing devices at near room temperature, obtaining quite different responsiveness. The microstructure of these hybrid materials is here systematically investigated by micro-Raman spectroscopy at 2.41 eV. The results show that regardless of the nominal C/Ti molar ratio (3.6 or 17.0) only the anatase phase of titania is formed. Theoretical calculations demonstrate that phonon confinement is fully responsible for the large blue-shift (∼10 cm−1) and broadening (∼20 cm−1) of the lowest-frequency Raman mode with respect to bulk anatase. The average size (4.3-5.0 nm) of TiO2 crystallites, resulting from Raman spectra fitting, is in excellent agreement with those inferred from transmission electron microscopy and X-ray diffraction measurements.  相似文献   

8.
A novel cobalt-tetraphenylporphyrin/reduced graphene oxide (CoTPP/RGO) nanocomposite was prepared by a π–π stacking interaction and characterized by ultraviolet–visible absorption spectroscopy (UV–vis), Fourier transform infrared spectroscopy (FTIR) and electrochemical impedance spectroscopy (EIS). The CoTPP/RGO nanocomposite exhibited high electrocatalytic activity both for oxidation and reduction of H2O2. The current response was linear to H2O2 concentration with the concentration range from 1.0 × 10−7 to 2.4 × 10−3 mol L−1 (R = 0.998) at the reductive potential of −0.20 V and from 1.0 × 10−7 to 4.6 × 10−4 mol L−1 (R = 0.996) at the oxidative potential of +0.50 V. The H2O2 biosensor showed good anti-interfering ability towards oxidative interferences at the oxidative potential of +0.50 V and good anti-interfering ability towards reductive interferences at the reductive potential of −0.20 V.  相似文献   

9.
Xiujie Bian  E. Jin 《Talanta》2010,81(3):813-83
Pt/polypyrrole (PPy) hybrid hollow microspheres were successfully prepared by wet chemical method via Fe3O4 template and evaluated as electrocatalysts for the reduction of hydrogen peroxide. The as-synthesized products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS), X-ray diffraction (XRD), inductive coupled plasma emission spectrum (ICP) and Fourier-transform infrared spectra (FTIR) measurements. The results exhibited that ultra-high-density Pt nanoparticles (NPs) were well deposited on the PPy shell with the mean diameters of around 4.1 nm. Cyclic voltammetry (CV) results demonstrated that Pt/PPy hybrid hollow microspheres, as enzyme-less catalysts, exhibited good electrocatalytic activity towards the reduction of hydrogen peroxide in 0.1 M phosphate buffer solution (pH = 7.0). The composite had a fast response of less than 2 s with linear range of 1.0-8.0 mM and a relatively low detection limit of 1.2 μM (S/N = 3). The sensitivity of the sensor for H2O2 was 80.4 mA M−1 cm−2.  相似文献   

10.
Some nanostructures are reported to possess enzyme-mimetic activities similar to those of natural enzymes. Herein, highly-dispersed Pt nanodots on Au nanorods (HD- PtNDs@AuNRs) with mimetic peroxidase activity were designed as an active electrode modifier for fabrication of a hydrogen peroxide (H2O2) electrochemical sensor. The HD-PtNDs@AuNRs were synthesized by a seed-mediated growth approach and confirmed by scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, and UV–vis spectroscopy. The electrochemical and catalytical performances of HD-PtNDs@AuNRs towards H2O2 reduction were investigated in detail by cyclic voltammetry and amperometry. The HD-PtNDs@AuNRs modified electrode displayed a high catalytic activity to H2O2 at −0.10 V (versus SCE), a rapid response within 5 s, a wide linear range of 2.0–3800.0 μM, a detection limit of 1.2 μM (S/N = 3), and a high sensitivity of 181 μA mM−1 cm−2. These results suggested a promising potential of fabricating H2O2 electrochemical sensor using HD- PtNDs@AuNRs.  相似文献   

11.
A novel bimediator amperometric sensor is fabricated for the first time by surface modification of graphite electrode with thionine (TH) and nickel hexacyanoferrate (NiHCF). The electrochemical behavior of the TH/NiHCF bimediator modified electrode was characterized by cyclic voltammetry, differential pulse voltammetry and chronoamperometry. The TH/NiHCF bimediator modified electrode exhibited a pair of distinct redox peaks for NiHCF and TH with formal potentials of 0.33 V and −0.27 V vs. SCE at a scan rate of 50 mV s−1 in 0.1 M NaNO3 and 0.1 M NH4NO3 respectively. The electrocatalytic activity of the bimediator modified electrode towards oxidation of gallic acid with NiHCF and reduction of hydrogen peroxide with TH was evaluated and it was observed that the modified electrode showed an electrocatalytic activity towards the oxidation of gallic acid in the concentration range of 4.99 × 10−6–1.20 × 10−3 M with a detection limit of 1.66 × 10−6 M (S/N = 3) and reduction of H2O2 in the concentration range of 1.67 × 10−6–1.11 × 10−3 M with a detection limit of 5.57 × 10−7 M (S/N = 3). The bimediator modified electrode was found to exhibit good stability and reproducibility.  相似文献   

12.
A highly sensitive NOx sensor was designed and developed by electrochemical incorporation of copper nanoparticles (CuNP) on single-walled carbon nanotubes (SWCNT)-polypyrrole (PPy) nanocomposite modified Pt electrode. The modified electrodes were characterized by scanning electron microscopy and energy dispersive X-ray analysis. Further, the electrochemical behavior of the CuNP-SWCNT-PPy-Pt electrode was investigated by cyclic voltammetry. It exhibited the characteristic CuNP reversible redox peaks at −0.15 V and −0.3 V vs. Ag/AgCl respectively. The electrocatalytic activity of the CuNP-SWCNT-PPy-Pt electrode towards NOx is four-fold than the CuNP-PPy-Pt electrode. These results clearly revealed that the SWCNT-PPy nanocomposite facilitated the electron transfer from CuNP to Pt electrode and provided an electrochemical approach for the determination of NOx. A linear dependence (r2 = 0.9946) on the NOx concentrations ranging from 0.7 to 2000 μM, with a sensitivity of 0.22 ± 0.002 μA μM−1 cm−2 and detection limit of 0.7 μM was observed for the CuNP-SWCNT-PPy-Pt electrode. In addition, the sensor exhibited good reproducibility and retained stability over a period of one month.  相似文献   

13.
The aim of this work was to determine structural parameters of the Y10−xLaxW2O21 (x=0-10) solid solution series and investigate their electric properties. Crystallographic data shows a gradual increase in symmetry with increasing La content, as the structure evolves from orthorhombic, Y10W2O21, towards the pseudo-cubic structure of Y5La5W2O21. The solubility limit of La2O3 was found to be 50% (x=5). Above this level two phases were observed, La6W2O15 and (La,Y)10+xW2−xO21−δ. The conductivity of Y rich samples was very low, with σ of the order 2×10−5-5×10−5 S cm−1 at 1000 °C, whilst ionic conductivity was observed for most La rich doped samples. The highest conductivity was observed for La10W2O21 and its doped analogues, at 1×10−3-5×10−3 S cm−1 at 1000 °C. Unit cell parameters were determined as a function of temperature from 0 to 1000°C, and thermal expansion of these materials was determined from temperature studies carried out at the Australian Synchrotron facility in Melbourne, Victoria, Australia.  相似文献   

14.
Based on the polyphosphonate-assisted coacervation of chitosan, a simple and versatile procedure for the encapsulation of proteins/enzymes in chitosan–carbon nanotubes (CNTs) composites matrix was developed. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), energy dispersive spectrum (EDS) mapping demonstrated the hemoglobin (Hb) uniformly distributed into chitosan–CNTs composites matrix. Raman measurements indicated the CNTs in composites matrix retained the electronic and structural integrities of the pristine CNTs. Fourier transform infrared (FT-IR), ultraviolet–visible (UV–vis) and circular dichroism (CD) spectroscopy displayed the encapsulated Hb preserved their near-native structure, indicating the polyphosphonate–chitosan–CNTs composites possessed excellent biocompatibility for the encapsulation of proteins/enzymes. Electrochemical measurements indicated the encapsulated Hb could directly exchange electron with the substrate electrode. Moreover, the modified electrode showed excellent bioelectrocatalytic activity for the reduction of hydrogen peroxide. Under optimum experimental conditions, the fabricated electrochemical sensor displayed the fast response (less than 3 s), wide linear range (7.0 × 10−7 to 2.0 × 10−3 M) and low detection limit (4.0 × 10−7 M) for the determination of hydrogen peroxide. This newly developed protocol was simple and mild and would certainly find extensive applications in biocatalysis, biosensors, bioelectronics and biofuel cells.  相似文献   

15.
In this paper, the photoelectrochemical behavior of graphene-TiO2 (G-TiO2) nanohybrids was investigated in the visible region and a new photoelectrochemical sensor for sensitive determination of nicotinamide adenine dinucleotide (NADH) was proposed. Under visible light, the G-TiO2 nanohybrids possessed enhanced photocurrent, which was nearly 5 times than that of pure TiO2 nanocrystals (NCs). Based on the enhanced photocurrent of G-TiO2 nanohybrids toward NADH, a new photoelectrochemical methodology for ultrasensitive determination of NADH was developed. The proposed sensor showed linearly enhanced photocurrent by increasing the NADH concentration from 1.0 × 10−8 to 2.0 × 10−3 M with a low detection limit of 3.0 × 10−9 M. Furthermore, this sensor exhibited good selectivity and stability towards NADH determination. This strategy opens up a new avenue for the application of graphene-based hybrids in the field of photoelectrochemical sensing and monitoring.  相似文献   

16.
A novel biomimetic sensor for rutin determination based on a dinuclear complex [MnIIIMnII(Ldtb)(μ-OAc)2]BPh4 containing an unsymmetrical dinucleating ligand, 2-[N,N-bis(2-pyridylmethyl)-aminomethyl]-6-[N-(3,5-di-tert-butyl-2-oxidoben-zyl)-N-(2-pyridylamino)aminomethyl]-4-methylphenol (H2Ldtb), as a manganese peroxidase mimetic was developed. Several parameters were investigated to evaluate the performance of the biomimetic sensor obtained after the incorporation of the dinuclear complex in a carbon paste. The best performance was obtained in 75:15:10% (w/w/w) of the graphite powder:Nujol:MnIIIMnII complex, 0.1 mol L−1 phosphate buffer solution (pH 6.0) and 4.0 × 10−5 mol L−1 hydrogen peroxide. The response of the sensor towards rutin concentration was linear using square wave voltammetry in the range of 9.99 × 10−7 to 6.54 × 10−5 mol L−1 (r = 0.9998) with a detection limit of 1.75 × 10−7 mol L−1. The recovery study performed with pharmaceuticals ranged from 96.6% to 103.2% and the relative standard deviation was 1.85% for a solution containing 1.0 × 10−3 mol L−1 rutin (n = 6). The lifetime of this biomimetic sensor was 200 days (at least 750 determinations). The results obtained for rutin in pharmaceuticals using the biomimetic sensor and those obtained with the official method are in agreement at the 95% confidence level.  相似文献   

17.
Jiao CX  Niu CG  Huan SY  Shen Q  Yang Y  Shen GL  Yu RQ 《Talanta》2004,64(3):637-643
The carbazole derivative, with an amino group in 9-position (9-methylacryloylamino carbazole (MAC), has been utilized to prepare a fluorescent sensor and used for the determination of NO2 based on the reaction between nitrite (NO2) and excess I to form I3, which can quench the fluorescence of carbazole derivative. MAC, as a fluorescent carrier, has a terminal double bond and is covalently immobilized on a quartz glass plate surface by photo-polymerization to prevent the leakage of the dye. The sensor shows sufficient repeatability, selectivity, operational lifetime of 8 weeks, and a fast response of less then 30 s. NO2 can be determined in the range between 1.0×10−6 and 1.0×10−4 mol l−1 with a detection limit of 8.0×10−7 mol l−1 at pH of 2.0. The quenching mechanism is discussed. Most commonly coexisting ions do not interfer with the NO2 assay.  相似文献   

18.
A novel amperometric biosensor based on self-assembling glutamate dehydrogenase (GLDH) and poly(amidoamine) dendrimer-encapsulated platinum nanoparticles (Pt-PAMAM) onto multiwall carbon nanotubes (CNTs) has been developed for the determination of glutamate. The formation of the self-assembled (GLDH/Pt-PAMAM)n/CNTs construction was investigated by ζ-potential and high resolution transmission electron microscopy (HRTEM). The results indicated the uniform growth of the layer-by-layer nanostructures onto carboxyl-functionalized CNTs. The electrocatalytic property of the (GLDH/Pt-PAMAM)n/CNTs modified electrode to glutamate in presence of NAD+ (β-nicotinamide adenine dinucleotide, 0.1 mM) was investigated at a low overpotential 0.2 V by electrochemical measurements. The results showed it had series of attractive characteristics, such as a large determination range (0.2-250 μM), a short response time (within 3 s), a high sensitivity (433 μA/mM−1 cm2) and good stability (85% remains after 4 weeks).  相似文献   

19.
A simple procedure was developed to prepare a glassy carbon electrode modified with single-wall carbon nanotubes (SWCNTs) and Os(III)-complex. The glassy carbon (GC) electrode modified with CNTs was immersed into Os(III)-complex solution (direct deposition) for a short period of time (60 s). 1,4,8,12-Tetraazacyclotetradecane osmium(III) chloride, (Os(III)LCl2)·ClO4, irreversibly and strongly adsorbed on SWCNTs immobilized on the surface of GC electrode. Cyclic voltammograms of the Os(III)-complex-incorporated-SWCNTs indicate a pair of well defined and nearly reversible redox couple with surface confined characteristic at wide pH range (1-8). The surface coverage (Γ) and charge transfer rate constant (ks) of the immobilized Os-complex on SWCNTs were 3.07 × 10−9 mol cm−2, 5.5 (±0.2) s−1, 2.94 × 10−9 mol cm−2, 7.3 (±0.3) s−1 at buffer solution with pH 2 and 7, respectively, indicate high loading ability of SWCNTs for Os(III) complex and great facilitation of the electron transfer between electroactive redox center and carbon nanotubes immobilized on the electrode surface. Modified electrodes showed higher electrocatalytic activity toward reduction of BrO3, IO3 and IO4 in acidic solutions. The catalytic rate constants for catalytic reduction bromate, periodate and iodate were 3.79 (±0.2) × 103, 7.32 (±0.2) × 103 and 1.75 (±0.2) × 103 M−1 s −1, respectively. The hydrodynamic amperometry of rotating modified electrode at constant potential (0.3 V) was used for nanomolar detection of selected analytes. Excellent electrochemical reversibility of the redox couple, good reproducibility, high stability, low detection limit, long life time, fast amperometric response time, wide linear concentration range, technical simplicity and possibility of rapid preparation are great advantage of this sensor.  相似文献   

20.
In this work, a highly selective and sensitive monohydrogen phosphate membrane sensor based on a molybdenum bis(2-hydroxyanil) acetylacetonate complex (MAA) is reported. The sensor shows a linear dynamic range between 1.0 × 10−1 and 1.0 × 10−7 M, with a nice Nernstian behavior (−29.5 ± 0.3 mV decade−1) in pH of 8.2. The detection limit of the electrode is 6.0 × 10−8 M (∼6 ppb). The best performance was obtained with a membrane composition of 32% poly(vinyl chloride), 58% benzyl acetate, 2% hexadecyltrimethylammonium bromide and 8% MAA. The sensor possesses the advantages of short response time, low detection limit and especially, very good selectivity towards a large number of organic and inorganic anions including salicylate, citrate, tartarate, acetate, oxalate, fluoride, chloride, bromide, iodide, sulfite, sulfate, nitrate, nitrite, cyanide, thiocyanate, perchlorate, metavanadate, and bicarbonate ions. The electrode can be used for at least 10 weeks without any considerable divergence in its slope and detection limit. It was used as an indicator electrode in potentiometric titration of monohydrogenphosphate ion with barium chloride. The proposed sensor was successfully applied to direct determination of monohydrogenphosphate in two fertilizer samples (NPK).  相似文献   

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