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1.
We report about the use of carbon paste electrode modified with kaolinite for analytical detection of trace lead(II) in domestic water by differential pulse voltammetry. Kaolinite clay was modified with tripolyphosphate (TPP) by impregnation method. The results show that TPP in kaolinite clay plays an important role in the accumulation process of Pb(II) on the modified electrode surface. The electroanalytical procedure for determination of Pb(II) comprised two steps: chemical accumulation of the analyte under open-circuit conditions, followed by electrochemical detection of the pre-concentrated species using differential pulse voltammetry. The analytical performance of this system has been explored by studying the effects of preconcentration time, carbon paste composition, pH, supporting electrolyte concentration, as well as interferences due to other ions. The calculated detection limit based on the variability of a blank solution (3sb criterion) for 10 measurements was 8.4 × 10−8 mol L−1, and the sensitivity determined from the slope of the calibration graph was 0.910 mol L−1. The reproducibility (RSD) for five replicate measurements at 1.0 mg L−1 lead level was 1.6%. The results indicate that this electrode is sensitive and effective for the determination of Pb2+.  相似文献   

2.
A graphene, chitosan and Fe3O4 nanoparticles (nano-Fe3O4) modified glassy carbon electrode (graphene-chitosan/nano-Fe3O4/GCE) was fabricated. The modified electrode was characterized by scanning electron microscope and electrochemical impedance spectroscopy. The electrochemical oxidation behavior of guanosine was investigated in pH 7.0 phosphate buffer solution by cyclic voltammetry and differential pulse voltammetry. The experimental results indicated that the modified electrode exhibited an electrocatalytic and adsorptive activities towards the oxidation of guanosine. The transfer electron number (n), transfer proton number (m) and electrochemically effective surface area (A) were calculated. Under the optimized conditions, the oxidation peak current was proportional to guanosine concentration in the range of 2.0 × 10−6 to 3.5 × 10−4 mol L−1 with the correlation coefficient of 0.9939 and the detection limit of 7.5 × 10−7 mol L−1 (S/N = 3). Moreover, the modified electrode showed good ability to discriminate the electrochemical oxidation response of guanosine, guanine and adenosine. The proposed method was further applied to determine guanosine in spiked urine samples and traditional Chinese medicines with satisfactory results.  相似文献   

3.
Santos LS  Landers R  Gushikem Y 《Talanta》2011,85(2):1213-1216
This work describes the in situ immobilization of Mn(II) phthalocyanine (MnPc) in a porous SiO2/SnO2 mixed oxide matrix obtained by the sol gel processing method. The chemically modified matrix SiO2/SnO2/MnPc, possessing an estimated amount of 8 × 10−10 mol cm−2 of MnPc on the surface, was used to prepare an electrode to analyze dissolved oxygen in water by an electrochemical technique. The electrode was prepared by mixing the material with ultrapure graphite and evaluated using differential pulse voltammetry. Dissolved O2 was reduced at −0.31 V with a limit of detection (LOD) equal to 7.0 × 10−4 mmol L−1. A mechanism involving four electrons in O2 reduction was determined by the rotating disk electrode technique.  相似文献   

4.
Zheng L  Xiong L  Zheng D  Li Y  Liu Q  Han K  Liu W  Tao K  Yang S  Xia J 《Talanta》2011,85(1):43-48
In this paper, a polydopamine (PDA) film is electropolymerized on the surface of bilayer lipid membrane (BLM) which is immobilized with horseradish peroxidase (HRP). The coverage of the PDA film on HRP/BLM electrode is monitored by electrochemical impedance spectroscopy (EIS). The electrocatalytic reduction of H2O2 at the PDA/HRP/BLM electrode is studied by means of cyclic voltammetry (CV). The biosensor has a fast response to H2O2 of less than 5 s and an excellent linear relationship is obtained in the concentration range from 2.5 × 10−7 to 3.1 × 10−3 mol L−1, with a detection limit of 1.0 × 10−7 mol L−1 (S/N = 3). The response current of BLM/HRP/PDA biosensor retains 84% of its original response after being stored in 0.1 mol L−1 pH 7.0 PBS at 4 °C for 3 weeks. The selectivity, repeatability, and storage stability of PDA/HRP/BLM biosensor are greatly enhanced by the coverage of polydopamine film on BLM.  相似文献   

5.
A modified carbon paste electrode based on multi-walled carbon nanotubes (MWCNTs) and 3-(4-methoxybenzylideneamino)-2-thioxothiazolodin-4-one as a new synthesized Schiff base was constructed for the simultaneous determination of trace amounts of Hg(II) and Pb(II) by square wave anodic stripping voltammetry. The modified electrode showed an excellent selectivity and stability for Hg(II) and Pb(II) determinations and for accelerated electron transfer between the electrode and the analytes. The electrochemical properties and applications of the modified electrode were studied. Operational parameters such as pH, deposition potential and deposition time were optimized for the purpose of determination of traces of metal ions at pH 3.0. Under optimal conditions the limits of detection, based on three times the background noise, were 9.0 × 10−4 and 6.0 × 10−4 μmol L−1 for Hg(II) and Pb(II) with a 90 s preconcentration, respectively. In addition, the modified electrode displayed a good reproducibility and selectivity, making it suitable for the simultaneous determination of Hg(II) and Pb(II) in real samples such as sea water, waste water, tobacco, marine and human teeth samples.  相似文献   

6.
BiFeO3 magnetic nanoparticles (BFO MNPs) are used as a catalyst to develop an ultrasensitive method for the determination of H2O2. It is found that BFO MNPs can catalyze the decomposition of H2O2 to produce OH radicals, which in turn oxidize the weakly fluorescent benzoic acid to a strongly fluorescent hydroxylated product with a maximum emission at 405 nm. This makes it possible to sensitively quantify traces of H2O2. Under optimized conditions, the fluorescence intensity is observed to be well linearly correlated with H2O2 concentration from 2.0 × 10−8 to 2.0 × 10−5 mol L−1 with a detection limit of 4.5 × 10−9 mol L−1 (S/N = 3). In addition, a selective method for glucose determination is developed by using both glucose oxidase and BFO MNPs, which has a linear range for glucose concentration from 1.0 × 10−6 to 1.0 × 10−4 mol L−1 with a detection limit of 5.0 × 10−7 mol L−1. These new methods have been successfully applied for the determination of H2O2 in rainwater and glucose in human serum samples.  相似文献   

7.
Due to the high performance of glassy carbon in the aspects of mechanical strength, electrical conductivity and high corrosion resistance, etc., glassy carbon has been widely used in the electrochemistry. A new form of glassy carbon, glassy carbon microsphere, was utilized to couple with ionic liquid in preparing a new electrochemiluminescent platform for Ru(bpy)3Cl2. Room temperature ionic liquid has been proposed to be very interesting and efficient pasting binder to replace the non conductive organic binders for the fabrication of composite paste electrode. Attributed to the special characteristics of glassy carbon microspheres and room temperature ionic liquid [N-octylpyridium tetrafluoroborate (OPFP)], this new electrochemiluminescent sensor exhibited excellent electrochemiluminescent performance in Ru(bpy)32+ solution. We first found that fentanyl citrate could increase the ECL of Ru(bpy)32+, hence an ECL approach was developed for the determination of fentanyl citrate based on this glassy carbon microspheres based electrochemiluminescent platform with high sensitivity. Under the optimized conditions, the enhanced electrochemiluminescent intensity versus fentanyl citrate concentration was linear in the range of 1.0 × 10−8 to 1.0 × 10−4 mol L−1 with a detection limit of 8.5 × 10−9 mol L−1, and the relative standard deviation for 1.0 × 10−6 mol L−1 fentanyl citrate was 1.90% (n = 10). This protocol has extended the application scopes of glassy carbon material and promoted the application of glassy carbon microspheres in electroanalysis.  相似文献   

8.
A simple electrochemical method was developed for the single and simultaneous determination of butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in food samples using square-wave voltammetry (SWV). A carbon composite electrode modified (MCCE) with copper (II) phosphate immobilized in a polyester resin was proposed. The modified electrode allowed the detection of BHA and BHT at potentials lower than those observed at unmodified electrodes. A separation of about 430 mV between the peak oxidation potentials of BHA and BHT in binary mixtures was obtained. The calibration curves for the simultaneous determination of BHA and BHT demonstrated an excellent linear response in the range from 3.4 × 10−7 to 4.1 × 10−5 mol L−1 for both compounds. The detection limits for the simultaneous determination of BHA and BHT were 7.2 × 10−8 and 9.3 × 10−8 mol L−1, respectively. In addition, the stability and repeatability of the electrode were determined. The proposed method was successfully applied in the simultaneous determination of BHA and BHT in several food samples, and the results obtained were found to be similar to those obtained using the high performance liquid chromatography method with agreement at 95% confidence level.  相似文献   

9.
Zhang Y  Zheng J 《Talanta》2008,77(1):325-330
An ionic liquid modified carbon paste electrode (IL/CPE) had been fabricated by using hydrophilic ionic liquid 1-amyl-3-methylimidazolium bromide ([AMIM]Br) as a modifier. The IL/CPE was characterized by scanning electron microscope and voltammetry. Electrochemical behavior of rutin at the IL/CPE had been investigated in pH 3.29 Britton-Robinson (B-R) buffer solution by cyclic voltammetry (CV) and square wave voltammetry (SWV). The experimental results suggested that the modified electrode exhibited an electrocatalytic activity toward the redox of rutin. The electron transfer coefficient (α) and the standard rate constant (ks) of rutin at the modified electrode were calculated. Under the selected conditions, the reduction peak current was linearly dependent on the concentration of rutin in the range of 4.0 × 10−8 to 1.0 × 10−5 mol L−1 (r = 0.9998), with a detection limit of 1.0 × 10−8 mol L−1 (S/N = 3). The relative standard deviation (R.S.D.) for six times successful determination of 8.0 × 10−7 mol L−1 rutin was 1.2%. The proposed method was applied to determine rutin in tablet and urine sample. In addition, the IL/CPE exhibited a distinct advantage of simple preparation, surface renewal, good reproducibility and good stability.  相似文献   

10.
Shuqing Dong  Yuzhi Fang 《Talanta》2009,80(2):809-303
In the paper, a new kind of vitamin B12 (acquo-cobalamine) chemically modified electrode was fabricated and applied in capillary zone electrophoresis coupled with amperometric detection (CZE-AD) for simultaneous determination of six antioxidants in fruits and vegetables. The catalytic electrochemical properties of the chemically modified electrode could obviously enhance oxidation peak heights responses by about five times to glutathione, ascorbic acid, vanillic acid, chlorogenic acid, salicylic acid, and caffeic acid compared with common carbon disk electrode. Furthermore, the effects of working electrode potential, pH and concentration of running buffer, separation voltage and injection time on CZE-AD were investigated. Under the optimum conditions, the six analytes could be completely separated and detected in a borate-phosphate buffer (pH 8.4) within 15 min. Their linear ranges were from 2.5 × 10−7 to 1.0 × 10−4 mol L−1 and the detection limits were as low as 10−8 mol L−1 magnitude (S/N = 3). The proposed method has been successfully employed to monitor the six analytes in practical samples with recoveries in the range 96.0-106.0% and RSDs less than 5.0%. Above results demonstrate that capillary zone electrophoresis coupled with electrochemical detection using vitamin B12 modified electrode as detector is of convenient preparation, high sensitivity, good repeatability, and could be used in the rapid determination of practical samples.  相似文献   

11.
Mehretie S  Admassie S  Hunde T  Tessema M  Solomon T 《Talanta》2011,85(3):1376-1382
A sensitive and selective method was developed for the determination of N-acetyl-p-aminophenol (APAP) and p-aminophenol (PAP) using poly(3,4-ethylenedioxythiophene) (PEDOT)-modified glassy carbon electrode (GCE). Cyclic voltammetry and differential pulse voltammetry were used to investigate the electrochemical reaction of APAP and PAP at the modified electrode. Both APAP and PAP showed quasireversible redox reactions with formal potentials of 367 mV and 101 mV (vs. Ag/AgCl), respectively, in phosphate buffer solution of pH 7.0. The significant peak potential difference (266 mV) between APAP and PAP enabled the simultaneous determination both species based on differential pulse voltammetry. The voltammetric responses gave linear ranges of 1.0 × 10−6-1.0 × 10−4 mol L−1 and 4.0 × 10−6-3.2 × 10−4 mol L−1, with detection limits of 4.0 × 10−7 mol L−1 and 1.2 × 10−6 mol L−1 for APAP and PAP, respectively. The method was successfully applied for the determination of APAP and PAP in pharmaceutical formulations and biological samples.  相似文献   

12.
An effective electrochemical sensor for the rapid and simultaneous determination of tramadol and acetaminophen based on carbon paste electrode (CPE) modified with NiFe2O4/graphene nanoparticles was developed. The structures of the synthesized NiFe2O4/graphene nanocomposite and the electrode composition were confirmed by X-ray diffraction (XRD) spectrometry, Fourier transform infrared (FT-IR) spectrometry and scanning electron microscopy (SEM). The peak currents of square wave voltammetry of tramadol and acetaminophen increased linearly with their concentration in the range of 0.01–9 μmol L−1. The detection limit for their determination was found to be 0.0036 and 0.0030 μmol L−1, respectively. The results show that the combination of graphene and NiFe2O4 nanoparticles causes a dramatic enhancement in the sensitivity of the sensor. The fabricated sensor exhibited high sensitivity and good stability, and would be valuable for the clinical assay of tramadol and acetaminophen.  相似文献   

13.
Titanium phosphate grafted on the surface of silica gel (devoted briefly as Si-TiPH) was synthesized and used as bulk modifier to fabricate a renewable three-dimensional chemically modified electrode. The Si-TiPH bulk modified carbon paste electrode was used for the selective determination of dopamine (DA) in the presence of ascorbic acid (AA). The modified electrode offers an excellent and stable response for the determination of DA in the presence of AA. The differential pulse voltammetry peak current was found to be linear with the DA concentration in the range 2 × 10−7 to 1 × 10−6 and 2 × 10−6 to 6 × 10−5 mol L−1. The detection limit of the proposed method in the presence of 2.0 × 10−5 M of AA was found to be 4.3 × 10−8 mol L−1 for DA determination. The proposed method was successfully applied for the determination of DA in injections.  相似文献   

14.
A simple and sensitive electroanalytical method is developed for the determination of lead by adsorptive stripping voltammetry (AdSV) in the presence of morin-5′-sulfonic acid (MSA) and sodium dodecyl sulfate (SDS). The Pb-MSA complex accumulates on the surface of a hanging mercury drop electrode (HMDE) and peak current is measured by square wave voltammetry (SWV). The complex is reduced at −0.48 V and peak current increases when low concentrations of SDS are added to the sample solution. The experimental variables pH, MSA concentration (CMSA); accumulation time (tacc); accumulation potential (Eacc), and SDS concentration (CSDS), as well as potential interferences, are investigated. Under the optimized conditions (pH 3.2; CMSA: 0.5 μmol L−1; tacc: 60 s; Eacc: −0.35 V, and CSDS: 20 μmol L−1), peak current is proportional to the concentration of Pb(II) over the 0.1-32.0 μg L−1 range, with a detection limit of 0.04 μg L−1. The relative standard deviation for a solution containing 5.0 μg L−1 of Pb(II) solution was 1.5% for seven successive assays. The method was validated by determining Pb(II) in synthetic sea water (ASTM D665) spiked with ICP multi-element standard solution and in certified reference water (GBW08607). Finally, the method was successfully applied to the determination of Pb(II) in tap water and sea water after UV digestion.  相似文献   

15.
In this paper, LaNi0.6Co0.4O3 (LNC) nanoparticles were synthesized by the sol–gel method, and the structure and morphology of LNC nanoparticles were characterized by X-ray diffraction spectrum, scanning electron microscopy and transmitting electron microscopy. And then, LNC was used to modify carbon paste electrode (CPE) without any adhesive to fabricate hydrogen peroxide and glucose sensor, and the results demonstrated that LNC exhibited strong electrocatalytical activity by cyclic voltammetry and amperometry. In H2O2 determination, linear response was obtained in the concentration range of 10 nM–100 μM with a detection limit of 1.0 nM. In glucose determination, there was the linear region of 0.05–200 μM with a detection limit of 8.0 nM. Compared with other reports, the proposed sensor also displayed high sensitivity toward H2O2 (1812.84 μA mM−1 cm−2) and glucose (643.0 μA mM−1 cm−2). Moreover, this prepared sensor was applied to detect glucose in blood serum and hydrogen peroxide in toothpaste samples with satisfied results, indicating its possibility in practical application.  相似文献   

16.
In this study, an hybrid material obtained by the intercalation of a gemini surfactant between the layers of smectite-type clay, was fully characterized by X-ray diffraction (XRD), infrared spectroscopy (FTIR) and N2 adsorption-desorption experiments (BET method). To ascertain the intercalation process of the starting clay by the dimeric surfactant, the permselectivity and ion exchange properties of the organoclay were investigated by ion exchange voltammetry using [Fe(CN)6]3− and [Ru(NH3)6]3+ as redox probes, by the means of a clay film-modified electrode. Due to its organophilic character, the surfactant-intercalated complex was evaluated as electrode modifier for the accumulation of methylparathion (MP) pesticide. The electroanalytical procedure involves two steps: preconcentration under open-circuit followed by voltammetric detection by square wave voltammetry: the peak current obtained (after 5 min preconcentration in 4 × 10−5 mol L−1 MP) on a glassy carbon electrode coated by a thin film of the modified clay was more than five times higher than that exhibited by the same substrate covered by a film of the pristine clay. This opens the way to the development of a sensitive method for the detection of the pesticide. Many parameters that can affect the stripping response (surfactant loading of the hybrid material, film composition, pH of the detection medium, preconcentration time, electrolysis potential and duration as well as some other instrumental parameters) were systematically investigated to optimize the sensitivity of the organoclay-modified electrode. After optimization, a linear calibration curve for MP was obtained in the concentration range from 4 × 10−7 to 8.5 × 10−6 mol L−1 in acetate buffer (pH 5), with a detection limit of 7 × 10−8 mol L−1 (signal-to-noise ratio equal to 3). The interference effect of various inorganic ions likely to influence the stripping determination of the pesticide was also examined, and the described method was applied to spring water analysis.  相似文献   

17.
Yongjin Zou  Lixian Sun  Fen Xu 《Talanta》2007,72(2):437-442
A Prussian Blue (PB)/polyaniline (PANI)/multi-walled carbon nanotubes (MWNTs) composite film was fabricated by step-by-step electrodeposition on glassy carbon electrode (GCE). The electrode prepared exhibits enhanced electrocatalytic behavior and good stability for detection of H2O2 at an applied potential of 0.0 V. The effects of MWNTs thickness, electrodeposition time of PANI and rotating rate on the current response of the composite modified electrode toward H2O2 were optimized to obtain the maximal sensitivity. A linear range from 8 × 10−9 to 5 × 10−6 M for H2O2 detection has been observed at the PB/PANI/MWNTs modified GCE with a correlation coefficient of 0.997. The detection limit is 5 × 10−9 M on signal-to-noise ratio of 3. To the best of our knowledge, this is the lowest detection limit for H2O2 detection. The electrode also shows high sensitivity (526.43 μA μM−1 cm−2) for H2O2 detection which is more than three orders of magnitude higher than the reported.  相似文献   

18.
Di J  Zhang F 《Talanta》2003,60(1):31-36
This paper described the determination of trace manganese using linear sweep voltammetry at a pretreatment glassy carbon electrode. The glassy carbon electrode pretreated by electrochemical method in the 0.1 mol l−1 NaOH solution greatly improved the electrode responsibility in the determination of manganese(II). The barrier to the detection of low manganese concentration was overcome by means of autocatalytic effect of manganese oxide deposited on the electrode in advance. Under the optimum experiments condition (0.04 mol l−1 NH3-NH4Cl buffer solution, pH 9.0), the linear range was 4×10−8 to 1×l0−6 mol l−1 Mn(II) for linear sweep voltammetry and 1×10−9 to 4×10−8 mol l−1 Mn(II) for convolution voltammetry. The relative standard deviation for 2×10−8 mol l−1 Mn(II) is 3.4%. The proposed method is simple, rapid, sensitive and selective. It had been applied to the determination of trace manganese in samples with satisfactory results.  相似文献   

19.
In this article a new coated platinum Cu2+ ion selective electrode based on 2-((2-(2-(2-(2-hydroxy-5-methoxybenzylideneamino)phenyl)disufanyl)phenylimino) methyl)-4-methoxyphenol Schiff base (L1) as a new ionophore is described. This sensor has a wide linear range of concentration (1.2 × 10−7-1.0 × 10−1 mol L−1) and a low detection limit of 9.8 × 10−8 mol L−1of Cu(NO3)2. It has a Nernstian response with slope of 29.54 ± 1.62 mV decade−1 and it is applicable in the pH range of 4.0-6.0 without any divergence in potentioal. The coated electrode has a short response time of approximately 9 s and is stable at least for 3.5 months. The electrode shows a good selectivity for Cu2+ ion toward a wide variety of metal ions. The proposed sensor was successfully applied for the determination of Cu2+ ion in different real and environmental samples and as indicator electrode for potentiometric titration of Cu2+ ion with EDTA.  相似文献   

20.
Enass M. Ghoneim 《Talanta》2010,82(2):646-652
A simple and precise square-wave adsorptive cathodic stripping voltammetry (SW-AdCSV) method has been described for simultaneous determination of Mn(II), Cu(II) and Fe(III) in water samples using a carbon paste electrode. In 0.1 mol L−1 acetate buffer (pH 5) containing 50 μmol L−1 of 2-(5′-bromo-2′-pyridylazo)-5-diethylaminophenol (5-Br-PADAP), Mn(II), Cu(II) and Fe(III) were simultaneously determined as metal-complexes with 5-Br-PADAP following preconcentration onto the carbon paste electrode by adsorptive accumulation at +1.0 V (vs. Ag/AgCl/3 M KCl). Insignificant interference from various cations (K+, Na+, Mg2+, Ca2+, Al3+, Bi3+, Sb3+, Se4+, Zn2+, Ni2+, Co2+, Cd2+, Pb2+, V5+, Ti4+ and NH4+), anions (HCO3, Cl, NO3−, SO42− and PO43−) and ascorbic acid was noticed. Limits of detection of 0.066, 0.108 and 0.093 μg L−1 and limits of quantitation of 0.22, 0.36 and 0.31 μg L−1 Mn(II), Cu(II) and Fe(III), respectively, were achieved by the described method. The described stripping voltammetry method was successfully applied for simultaneous determination of Mn(II), Cu(II) and Fe(III) in ground, tap and bottled natural water samples.  相似文献   

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