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1.
The silver nanoparticles were prepared on the glassy carbon (GC) electrode, modified with p-iso propyl calix[6]arene, by preconcentration of silver ions in open circuit potential and followed by electrochemical reduction of silver ions. The stepwise fabrication process of Ag nanoparticles was characterized by scanning electron microscopy and electrochemical impedance spectroscopy. The prepared Ag nanoparticles were deposited with an average size of 70 nm and a homogeneous distribution on the surface of electrode. The observed results indicated that the presence of calixarene layer on the electrode surface can control the particle size and prevent the agglomeratione and electrochemical deposition is a promising technique for preparation of nanoparticles due to its easy-to-use procedure and low cost of implementation. Cyclic voltammetry experiments showed that Ag nanoparticles had a good catalytic ability for the reduction of hydrogen peroxide (H2O2). The effects of p-isopropyl calix[6]arene concentration, applied potential for reduction of Ag+, number of calixarene layers and pH value on the electrocatalytic ability of Ag nanoparticles were investigated. The present modified electrode exhibited a linear range from 5.0 × 10−5 to 6.5 × 10−3 M and a detection limit 2.7 × 10−5 M of H2O2 (S/N = 3) using amperometric method.  相似文献   

2.
In this work, the metal oxide and biopolymer nanocomposites on multiwalled carbon nanotubes (MWCNT) were prepared using a simple sonochemical method. The hexagonal nanorods of zinc oxide (ZnO NR) were synthesized by probe sonication (frequency = 20 kHz, amplitude = 50) method and were integrated on ultrasonically functionalized MWCNT-cellulose nanocrystals (MWCNT-CNC) for the first time. The stable hemin bio-composites also were prepared using the bath sonication (37 kHz of frequency, 150 W of power) method, and was used for the selective and ultrasensitive electrochemical detection of H2O2. The UV–Vis spectroscopy studies confirmed the presence of native hemin on MWCNT-CNC/ZnO NR nanocomposite. Cyclic voltammetry studies revealed that an enhanced redox electrochemical behaviour of hemin was observed on hemin immobilised MWCNT-CNC/ZnO NR nanocomposite than that of other hemin modified electrodes. Also, the MWCNT-CNC/ZnO NR/hemin modified SPCE showed 2.3 folds higher electrocatalytic activity with a lower reduction potential (−0.2 V) towards H2O2 than that of other investigated hemin modified electrodes including hemin/MWCNT and hemin/CNC-ZnO. The fabricated biosensor displayed a stable amperometric response (-0.2 V vs Ag/AgCl) in the linear concentration of H2O2 ranging up to 4183.3 µM with a lower detection limit of 4.0 nM.  相似文献   

3.
A simple and sensitive chemiluminescence (CL) method coupled with flow-injection technique is proposed to determine naproxen (NAP). The method is based upon the enhancement of the weak CL signal arising from the reaction of Ce(IV) and Na2S2O4 with Eu3+ to form the Eu3+-Ce(IV)-Na2S2O4 system. The CL intensity was significantly increased by the introduction of NAP into this system in the presence of silver nanoparticles (Ag NPs). Examination of the recorded UV–vis spectra and fluorescence spectra indicated that the energy of the intermediate SO2*, which originated from the redox reaction of Ce(IV) and Na2S2O4, was transferred to Eu3+ via NAP and that the process was accelerated by Ag NPs due to their catalytic activity. Under the optimum conditions, the CL intensity was increased with increasing NAP concentration and the correlation was linear (r = 0.9992) over the NAP concentration range of 1–420 ng mL−1. The limit of detection (LOD) was 0.11 ng mL−1 with a relative standard deviation (RSD) of 1.15% for 5 replicate determinations of 200 ng mL−1 NAP. The method was successfully applied to determine NAP in pharmaceutical and biological samples.  相似文献   

4.

Abstract  

Ag nanoparticles/graphene nanosheet (AgNPs/GN) composites have been rapidly prepared by a one-pot microwave-assisted reduction method, carried out by microwave irradiation of a N,N-dimethylformamide (DMF) solution of graphene oxide (GO) and AgNO3. Several analytical techniques including UV–vis spectroscopy, FT-IR spectroscopy, Raman spectroscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM) have been used to characterize the resulting AgNPs/GN composites. It suggests that such composites exhibit good catalytic activity toward reduction of hydrogen peroxide (H2O2), leading to a H2O2 sensor with a fast amperometric response time of less than 2 s. The linear detection range is estimated to be from 0.1 to 100 mM (r = 0.999), and the detection limit is estimated to be 0.5 μM at a signal-to-noise ratio of 3.  相似文献   

5.
A fluorophotometric method for the determination of hydrogen peroxide (H2O2) using fluorescin was developed. This method was based on the oxidative reaction of fluorescin, a colorless, non-fluorescent lactoid fluorescein, by H2O2 to give highly fluorescein fluorescence emission. In the determination of H2O2, the calibration curve exhibited linearity over the H2O2 concentration range of 1.5–310 ng mL−1 at an emission wavelength of 525 nm with an excitation of 500 nm and with relative standard deviations (n = 6) of 2.51%, 2.48%, and 1.31% for 3.1 ng mL−1, 30.8 ng mL−1, and for 308 ng mL−1 of H2O2, respectively. The detection limit for H2O2 was 1.9 ng mL−1 six blank determinations was performed (ρ = 6). This proposed method was applied to detection of other reactive oxygen species and nitrogen species (ROS/RNS) such as singlet oxygen (1O2), hydroxyl radical (OH), peroxynitrite (ONOO) etc., and it was possible to detect them with a high sensitivity. In addition, this proposed method was applied to the recovery tests of H2O2 in calf serum, human saliva, rain water, and wheat noodles; the results were satisfactory.  相似文献   

6.
This study synthesized Fe3O4 nanoparticles of 30–40 nm by a sonochemical method, and these particles were uniformly dispersed on the reduced graphene oxide sheets (Fe3O4/RGO). The superparamagnetic property of Fe3O4/RGO was evidenced from a saturated magnetization of 30 emu/g tested by a sample-vibrating magnetometer. Based on the testing results, we proposed a mechanism of ultrasonic waves to explain the formation and dispersion of Fe3O4 nanoparticles on RGO. A biosensor was fabricated by modifying a glassy carbon electrode with the combination of Fe3O4/RGO and hemoglobin. The biosensor showed an excellent electrocatalytic reduction toward H2O2 at a wide, linear range from 4 × 10?6 to 1 × 10?3 M (R2 = 0.994) as examined by amperometry, and with a detection limit of 2 × 10?6 M. The high performance of H2O2 detection is attributed to the synergistic effect of the combination of Fe3O4 nanoparticles and RGO, promoting the electron transfer between the peroxide and electrode surface.  相似文献   

7.
An efficient biosensing substrate based on ZrO2/DNA-derivated polyion complex (PIC) membrane has been developed for the determination of hydrogen peroxide (H2O2) in this study. To fabricate such a PIC membrane, ZrO2 nanoparticles were initially electrodeposited on the bare gold electrode (ZrO2/Au), and deoxyribonucleic acid (DNA)-doped hemoglobin mixture was then assembled onto the ZrO2/Au surface. The double-strand DNA provided a biocompatible microenvironment for the immobilization of biomolecules, greatly amplified the surface coverage of biomolecules on the electrode surface, and improved the sensitivity of the biosensor. The fabricated procedure of the proposed biosensor was characterized by cyclic voltammetry, electrochemical impedance spectroscopy, and atomic force microscopy. The performance and factors influencing the performance of the biosensor were also evaluated. Under optimal conditions, the developed biosensor exhibited a well-defined electrochemical behavior toward the reduction of H2O2 ranging from 1.1 μM to 2.3 mM with a detection limit of 0.5 μM (S/N = 3). The biosensor was applied to the determination of H2O2 in milk with satisfactory results. It is important to note that the PIC membrane provided an alternative substrate for the immobilization of other proteins.  相似文献   

8.
In this paper, an amperometric electrochemical biosensor for the detection of hydrogen peroxide (H2O2), based on gold nanoparticles (GNPs)/thionine (Thi)/GNPs/multi-walled carbon nanotubes (MWCNTs)-chitosans (Chits) composite film was developed. MWCNTs-Chits homogeneous composite was first dispersed in acetic acid solution and then the GNPs were in situ synthesized at the composite. The mixture was dripped on the glassy carbon electrode (GCE) and then the Thi was deposited by electropolymerization by Au-S or Au-N covalent bond effect and electrostatic adsorption effect as an electron transfer mediator. Finally, the mixture of GNPs and horseradish peroxidase (HRP) was assembled onto the modified electrode by covalent bond. The electrochemical behavior of the modified electrode was investigated by scanning electron microscope, cyclic voltammetry and chronoamperometry. This study introduces the in situ-synthesized GNPs on the other surface of the modified materials in H2O2 detection. The linear response range of the biosensor to H2O2 concentration was from 5 × 10−7 mol L−1 to 1.5 × 10−3 mol L−1 with a detection limit of 3.75 × 10−8 mol L−1 (based on S/N = 3).  相似文献   

9.
Small size (25 nm) Li2B4O7 nanoparticles doped with different concentrations of Cu, Ag and co-doped with Cu, Ag were prepared by solid state sintering at 700 °C. The crystalline phase and particle sizes analysis were carried out by XRD and TEM. FTIR study reveals the formation of vibrational bonds at 1600–1200 cm−1, 1500–700 cm−1, 950–870 cm−1 and 870–415 cm−1. The kinetic parameters of the TL glow curves were evaluated using CGCD procedure in R-software. The CW-OSL decay curves were fitted with third order exponential decay curves and photoionization cross sections of each component were evaluated. The lifetime of the main TL dosimetric peak were also calculated to check the stability of the signal. Dose responses of the synthesized Li2B4O7 nanoparticles for both the TL and CW-OSL were studied in the range of 0.02 mGy to50 Gy and found to be linear upto this range. Fading of the CW-OSL decay curves were also studied. The MDD of the synthesized samples were also calculated and observed to be 15 μGy.  相似文献   

10.
In this article, we have reported on the synthesis of ultra-highly concentrated (5.88 M), well-stable Ag nanoparticles (AgNPs). The AgNPs were formed by hydrothermal heat treatment of an aqueous solution of poly [(2-ethyldimethylammonioethyl methacrylate ethyl sulfate)-co-(1-vinylpyrrolidone)] (PQ11), a kind of cationic polyeletrolyte, in the presence of AgNO3 powder at 170 °C, without the additional step of introducing other reducing agents and protective agents. Transmission electron microscopy (TEM) observations reveal that the as-formed AgNPs mainly consist of small nanoparticles about 10 nm in diameter. Most importantly, it was found that such dispersion can form stable films on bare electrode surfaces and the AgNPs contained therein still exhibit notable catalytic performance for reduction of hydrogen peroxide (H2O2). This H2O2 sensor has a fast amperometric response time of less than 3 s. Its linear range is estimated to be from 0.1 to 60 mM (r = 0.993), and the detection limit is estimated to be 1.6 μM at a signal-to-noise ratio of 3.  相似文献   

11.
Metal nanoparticles have many potential technological applications. Biological routes to the synthesis of these particles have been proposed including production by vascular plants, known as phytoextraction. While many studies have looked at metal uptake by plants, particularly with regard to phytoremediation and hyperaccumulation, few have distinguished between metal deposition and metal salt accumulation. This work describes the uptake of AgNO3, Na3Ag(S2O3)2, and Ag(NH3)2NO3 solutions by hydroponically grown Brassica juncea and the quantitative measurement of the conversion of these salts to silver metal nanoparticles. Using X-ray absorption near edge spectroscopy (XANES) to determine the metal speciation within the plants, combined with atomic absorption spectroscopy (AAS) for total Ag, the quantity of reduction of AgI to Ag0 is reported. Transmission electron microscopy (TEM) showed Ag particles of 2–35 nm. The factors controlling the amount of silver accumulated are revealed. It is found that there is a limit on the amount of metal nanoparticles that may be deposited, of about 0.35 wt.% Ag on a dry plant basis, and that higher levels of silver are obtained only by the concentration of metal salts within the plant, not by deposition of metal. The limit on metal nanoparticle accumulation, across a range of metals, is proposed to be controlled by the total reducing capacity of the plant for the reduction potential of the metal species and limited to reactions occurring at an electrochemical potential greater than 0 V (verses the standard hydrogen electrode).  相似文献   

12.
In the luminol-O2 ECL system, O2 as an endogenous coreactant has the advantages of non-toxicity and stability. Improving the efficiency to generate radicals of O2 is a challenge currently. In this work, a strategy combining physical method - ultrasound and nanomaterial with unique physicochemical properties was designed to enhance the ECL signal of luminol-O2 system. Specifically, high-intensity focused ultrasound (HIFU) pretreatment as a non-invasive method could generate ROS (H2O2, O2•−, OH•, 1O2) in situ, triggering and boosting the ECL signal of luminol. In addition, 1T/2H MoS2 with excellent catalytic activity could catalyze the H2O2 produced in situ, accelerate the oxidation of luminol and further enhance the ECL response. At the same time, combined with the catalytic hairpin assembly (CHA) reaction, the constructed ECL biosensing platform showed excellent performance for the detection of miRNA-155. The concentration range of 0.1 fM ∼ 1 nM with the detection limit as low as 0.057 fM were obtained. Furthermore, the ECL biosensor was also successfully applied to the determination of miRNA-155 in human serum samples. The established ECL sensing platform opens up a promising method for the detection of clinical biomarkers.  相似文献   

13.
In the paper, a chemiluminescence (CL) system was developed based on the catalytical effect of diperiodatocuprate (III) (DPC) on the 1,10-phenanthroline (phen)/hydrogen peroxide (H2O2) in the presence of cetyltrimethylammonium bromide (CTAB). The effects of experimental conditions were investigated. Meanwhile the increase of CL intensity of the DPC/phen/H2O2/CTAB system is proportional to the concentration of phen in the range of low concentration. The linear range of the calibration curve is 5.0 × 10−9–1.0 × 10−6 mol L−1, and the corresponding detection limit is 1.9 × 10−9 mol L−1. The effects of phenolic compounds (PCs) on the system were investigated. Hydroquinone was used as an example to investigate the application of the CL system to the determination of PCs. The quenched CL intensity is linearly related to the logarithm of concentration of hydroquinone. The linear range of the calibration curve is 2.5 × 10−9–1.0 × 10−5 g mL−1, and the corresponding detection limit is 1.8 × 10−9 g mL−1. This phen and hydroquinone can be synchronously determined. The method was applied to the determination of hydroquinone in water samples and the recoveries were from 92% to 106%.  相似文献   

14.
《Ultrasonics sonochemistry》2014,21(6):1958-1963
A simple sonochemical route was developed for the preparation of gold nanoparticles/boron nitride sheets (AuNPs/BNS) nanocomposites without using reducing or stabilizing agents. Transmission electron microscopy, scanning electron microscopy, X-ray diffraction, and UV–vis absorption spectra were used to characterize the structure and morphology of the nanocomposites. The experimental results showed that AuNPs with approximately 20 nm were uniformly attached onto the BNS surface. It was found that the AuNPs/BNS nanocomposites exhibited good catalytic activity for the reduction of H2O2. The modified electrochemical sensor showed a linear range from 0.04 to 50 mM with a detection limit of 8.3 μM at a signal-to-noise ratio of 3. The findings provide a low-cost approach to the production of stable aqueous dispersions of nanoparticles/BNS nanocomposites.  相似文献   

15.
Ag nanoparticles on SiO2/Si surfaces synthesized using the Tollen's reagent and a subsequent acid-etching were characterized using X-ray photoelectron spectroscopy (XPS). Combining the reduction of the Tollen's reagent and the chemical etching, one can create naked Ag nanoparticles with various sizes in the size range below ∼10 nanometers (nm). The reduced particle size by the chemical etching was identified using positive core level shifts with increasing etching time. Ag nanoparticles smaller than ∼3 nm undergo a reversible oxidation and reduction cycle by reacting with H2O2/H2O and a subsequent heating under vacuum to 150 °C, which was not found for the bulk counterparts and larger particles, demonstrating unique chemical properties of nanoparticles compared to the bulk counterparts.  相似文献   

16.
Nano-sized Al3+-doped V2O5 cathode materials, Al0.2V2O5.3−δ , were prepared by an oxalic acid assisted sol–gel method at 350 °C (sample A) and 400 °C (sample B). X-ray diffraction confirmed that samples A and B were pure phase Al0.2V2O5.3−δ with an orthorhombic structure close to that of V2O5. Scanning electron microscopy showed that sample A was in nanoscale with a mean particle size about 50 nm. Cyclic voltammetry showed the good electrochemical and structural reversibility of the Al0.2V2O5.3−δ nanoparticles during the Li+ insertion/extraction process. The Al0.2V2O5.3−δ nanoparticles exhibited excellent charge–discharge cycling performance and rate capability compared to that of bulky V2O5 electrodes. For instance, the materials delivered a reversible specific capacity about 180 mAh g−1 (sample A) and 150 mAh g−1 (sample B), in the potential window of 4.0–2.0 V at the current density of 150 mA g−1. The Al0.2V2O5.3−δ nanoparticles in particular showed almost no capacity fading for at least 50 cycles.  相似文献   

17.
Lithium borate (LBO) single crystals doped with Cu and Ag (0.25 mol% each) (Li2B4O7:Cu,Ag) are grown by the Czochralski method. The thermoluminescence readout on Li2B4O7:Cu,Ag crystals showed three glow peaks at~375, 441 and 516 K for the heating rate of 1  K/s. The thermoluminescence sensitivity of the grown Li2B4O7:Cu,Ag single crystals is found to be 5 times TLD-100 and a linear dose response in the range 1 mGy to 1 kGy. The glow curve deconvolution reveals nearly first order kinetics for all the three peaks with trap depths 0.77, 1.25 and 1.34 eV respectively and corresponding frequency factors 1.6×109, 1.3×1013 and 6.8×1011 s?1. The continuous wave optically stimulated luminescence (CW-OSL) measurements were performed on the LBO:Cu,Ag single crystals using blue light stimulation. The traps responsible for the three thermoluminescence peaks in Li2B4O7:Cu,Ag are found to be OSL sensitive. The qualitative correlation between TL peaks and CW-OSL response is established. The photoluminescence studies show that in case of co-doping of Ag in LBO:Cu the emission at 370 nm in Cu states dominates over the transitions in Ag states implying doping of Ag plays a role as sensitizer when co-doped with Cu and increases overall emission.  相似文献   

18.
《Current Applied Physics》2020,20(12):1416-1423
Recently, spinel-type binary metal oxides have attracted enormous interest in energy storage devices. In supercapacitors improving energy density is still challenging task and the composite nanostructures are found to address this issue in some extent. Herein, a composite nanostructure based on ZnCo2O4/CdS was synthesized on nickel foam using hydrothermal and successive ionic layer adsorption and reaction (SILAR) methods. A hydrothermally synthesized ZnCo2O4 nanoflowers were coated by CdS nanoparticles by varying SILAR cycles and studied its electrochemical performance. The ZnCo2O4/CdS nanostructured electrode with optimized four SILAR cycles of CdS coating exhibited a high areal capacity, energy density and power density of 2658 mCcm−2, 517 μWhcm−2 and 17.5 mWcm−2 at 25 mA, which is higher than pristine ZnCo2O4. This work show ZnCo2O4/CdS nanostructure is a favorable electrode for supercapacitors.  相似文献   

19.
We present in this work the direct observation of HO2 radicals after irradiation of benzene C6H6 at 248 nm in the presence of O2. HO2 radicals have been unambiguously identified using the very selective and sensitive detection of continuous wave cavity ring-down spectroscopy (cw-CRDS) coupled to a laser photolysis reactor. HO2 radicals were detected in the first vibrational overtone of the OH stretch at 6638.20 cm-1, using a DFB diode laser. This reaction might be important because 248 nm photolysis of H2O2 has often been used in the past for studying the OH-initiated degradation of C6H6, often using a large excess of C6H6 over H2O2. The possible importance of the title reaction with respect to these former laboratory studies has been quantified through comparison with HO2 signals obtained from 248 nm photolysis of H2O2: one obtains under our conditions (excess O2 and total pressure of 6.6 kPa helium) from the 248 nm irradiation of identical initial concentrations [C6H6]=[H2O2] the following relative initial radical concentrations: [HO2 ]=(0.28±0.05)×[OH]. Experiments with various O2 concentrations have revealed that the origin of the HO2 radicals is not the reaction of H-atoms with O2, but must originate from the reaction of O2 with excited C6H6 *. The quantum yield of C6H6 * formation has been deduced to ϕ=0.2±0.1. PACS  42.62.Fi; 82.20.Pm; 82.33.Tb  相似文献   

20.
Defective graphene nanosheets (dGN4V) with 5-9, 5-8-5, and point defects were synthesised by a sonoelectrochemical method, where a potential of 4 V (vs. Ag/AgCl) was applied to drive the rapid intercalation of phosphate ions between the layers of the graphite foil as a working electrode. In addition to these vacancies, double vacancy defects were also created when the applied potential was increased to 8 V (dGN8V). The defect density of dGN8V (2406 μm−2) was higher than that of dGN4V (1786 μm−2). Additionally, dGN8V and dGN4V were applied as catalysts for the hydrogen peroxide reduction reaction (HPRR). The mass activity of dGN8V (1.31 × 10−2 mA·μg−1) was greater than that of dGN4V (1.17 × 10−2 mA·μg−1) because of its high electrochemical surface area (ECSA, 1250.89 m2·g−1) and defect density (ND, 2406 μm−2), leading to low charge transfer resistance on the electrocatalytic interface. The ECSA and ND of dGN4V were 502.7 m2·g−1 and 1786 μm−2, respectively. Apart from its remarkable HPRR activity, the cost-effective dGN8V catalyst also showed potential as an amperometric sensor for the determination of H2O2.  相似文献   

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