A new sensitive adsorptive voltammetric method was described for the determination of zirconium at a carbon paste electrode (CPE) in the presence of alizarin complexone (ALC). Optimal analytical conditions are: 1.0?0...A new sensitive adsorptive voltammetric method was described for the determination of zirconium at a carbon paste electrode (CPE) in the presence of alizarin complexone (ALC). Optimal analytical conditions are: 1.0?0-6 or 5.0?0-7 mol/L ALC, 0. 20 mol/L HAC-NaAc (pH 4.3), accumulation for 60 s at 0 V (vs. SCE), and linear scanning from 0 V to 1.0 V at 250 mV/s. The peak potential of the complex is at 0.81 V. By using a model JP-303 polarographic analyzer, 2.0?0-10 mol/L (S/N=3) zirconium can be detected with a 90 s accumulation, when the 2nd-order derivative linear sweep technique is used, and the linear range is 6.0?0-10-2.0?0-8 mol/L (5.0?0-7 mol/L ALC) and 2.0?0-8-2.0?0-7 mol/L (1.0?0-6 mol/L ALC), respectively. The developed method was applied to the determination of trace zirconium in the ore samples with satisfactory results.展开更多
A sensitive method is described for the determination of trace antimony based on the antimony-bromopyrogallol red (BPR) adsorption at a carbon paste electrode (CPE). Three steps were involved in the overall analysis: ...A sensitive method is described for the determination of trace antimony based on the antimony-bromopyrogallol red (BPR) adsorption at a carbon paste electrode (CPE). Three steps were involved in the overall analysis: preconcentration,reduction and stripping. Optimal conditions were found to be an electrode containing 25% paraffin oil and 75% high purity graphite powder as working electrode;a 0.10 mol/L HCl solution containing 40 μmol/L BPR as accumulation medium;a 0.20 mol/L HCl solution as reduction and stripping electrolyte;accumulation time,150 s;reduction potential and time,-0.50 V,60 s;scan range from -0.50 to 0.20 V. Interferences by other ions were studied as well. The detection limit was found to be 0.5 nmol/L for 150 s preconcentration. The linear range was from 1.0 nmol/L to 0.50 μmol/L. Application of the proposed method to the determination of antimony in water and human hair samples gave good results.展开更多
This study presents the elaboration of a simple and cheap electrode made by carbon paste introduced into a cavity of electrode body, and used for the lead traces determination in tap water. A potentiostatic pre-electr...This study presents the elaboration of a simple and cheap electrode made by carbon paste introduced into a cavity of electrode body, and used for the lead traces determination in tap water. A potentiostatic pre-electrolysis at constant voltage enables the reduction of the lead (Pb2+) and the accumulation of the metallic lead at and into the carbon paste;the reoxidation of the Pb (Linear sweep voltammetry) leads to the anodic striping peak. The effect of the main operating parameters on the shape of the peak and the magnitude of the current was examined and their optimal values were determined. Then calibration was achieved and the method was successfully applied (using all the optimized parameters) to the determination of lead in water, with a detection limit of 0.138 μg·L-1. Compared to other methods (ICP-AES for example), the proposed method offers a satisfactory detection limit of the Pb2+ (0.138 μg·L-1) because of the important specific area of the carbon paste electrode, for a significantly lower cost. Besides, there is no observed loss in the electrode answer in terms of peak current, which means that there is no any irreversible steps nor deactivation of the electrode, even after ten successive measurements;only reduction of the lead followed by the deposit oxidation was observed at the electrode.展开更多
A novel method was described for the determination of ultra trace amount of scandium based on the cathodic adsorptive voltammetry of the mix-polynuclear complex of scandium-calcium-alizarin red S at a carbon paste ele...A novel method was described for the determination of ultra trace amount of scandium based on the cathodic adsorptive voltammetry of the mix-polynuclear complex of scandium-calcium-alizarin red S at a carbon paste electrode (CPE). The 2nd-order derivative linear scan voltammograms of the adsorbed complex were recorded by model JP-303 polarographic analyzer from 0.0 to -1.0 V (vs. SCE). The experimental conditions of the working procedure were optimized. The results show that the complex can be adsorbed on the surface of the CPE, yielding one peak at -0.61 V, corresponding to the reduction of the alizarin red S in the mix-polynuclear complex at the electrode. The detection limit of Sc^(3+) is 1.0×10^(-10) mol·L^(-1) for 3 min of accumulation time. The procedure was successfully applied to the determination of trace amount of scandium in the sample ores.展开更多
A simple method for anodic stripping voltammetric determination of nitrite using carbon paste electrode modified with biomolecular chitosan, is described. In this method, the electrode is activated electrochemically b...A simple method for anodic stripping voltammetric determination of nitrite using carbon paste electrode modified with biomolecular chitosan, is described. In this method, the electrode is activated electrochemically by scanning 5 replicates over the potential range from +500 to +1400 mV immersing in 0.5 M HCl solution. Following this step, the nitrite sample containing 0.1 M KCl is preconcentrated on the activated electrode at +500 mV for 30 s. The deposited anions are then oxidized by different modes of sweep in the oxidation direction. Chemical and electrical parameters affecting the voltammetric measurements are optimized. The peak current is linear proportional to the NO2- concentration within the range 0.41 - 4.1 μg/ml, with detection limit 0.187 μg/m using differential pulse mode. The relative standard deviation is 0.285% for 2.46 μg/ml (five replicates). No interference is observed due to oxygen dissolved in the sample so that nitrogen purging is not needed in this case. The result obtained by the modified electrode is more accurate and selective than the unmodified electrode.展开更多
A carbon paste electrode modified with multi-walled carbon nanotubes (MWCNT) was prepared and the determination of ultra trace amount of zirconium based on the anodic adsorptive voltammetry of the zirconium-calcium-al...A carbon paste electrode modified with multi-walled carbon nanotubes (MWCNT) was prepared and the determination of ultra trace amount of zirconium based on the anodic adsorptive voltammetry of the zirconium-calcium-alizarin red S mix-polynuclear complex is described in this paper for the first time. The results showed that the sensitivity and the selectivity of the method are excellent. The second de-rivative linear scan voltammograms of the complex were recorded by polarographic analyzer from 200 to 1200 mV (vs. SCE) and it was found that the complex can be adsorbed on the surface of the electrode, yielding a peak at about 840 mV, corresponding to the oxidation of ARS in the complex. The peak cur-rent increases linearly with Zr (IV) concentration in the range of 6.0×10-12―6.0×10-11 mol·L-1 (accumu-lation time 120 s), 6.0×10-11―2.0×10-9 mol·L-1 (accumulation time 90 s) and 2.0×10-9―1.0×10-7 mol·L-1 (accumulation time 60 s) and the detection limit (S/N = 3) is 2.0×10-12 mol·L-1 (accumulation time 180 s). The procedure has been successfully applied to the determination of zirconium in the ore samples.展开更多
Voltammetry using solid electrodes usually suffers from the contamination due to the deposition of the redox products of analytes on the electrode surface. The contamination has resulted in poor reproducibility and ov...Voltammetry using solid electrodes usually suffers from the contamination due to the deposition of the redox products of analytes on the electrode surface. The contamination has resulted in poor reproducibility and overelaborate operation procedures. The use of the chemical catalysis of oxidant on the reduction product of analyte not only can eliminate the contamination of analyte to solid electrodes but also can improve the faradaic response of analyte. This work introduced both the catalysis of oxidant K2S2O8 and the enhancement of surfactant Triton X-100 on the faraday response of amiodarone into an adsorptive stripping voltammetry at a carbon paste electrode for the determination of amiodarone. The method exhibits high sensitivity, good reproducibility and simple operation procedure. In 0.2 mol·L^-1 HOAc-NaOAc buffer (pH=5.3) containing 2.2×10^-2 mol·L^-1 K2S2O8 and 0.002% Triton X-100, the 2.5th-order derivative stripping peak current of the catalytic wave at 0.3 V (vs. Ag/AgCl) is rectilinear to amiodarone concentration in the range of 2.0×10^-10-2.3×10^-8 mol·L^-1 with a detection limit of 1.5×10^-10 mol·L^-1 after accumulation at 0 V for 30 s.展开更多
Ultra trace determination of lantanum(Ⅲ) has been studied by adsorptive stripping voltammetry methods using an alizarin S as complexing agent and carbon paste electrode as working electrode. The electrode was made ...Ultra trace determination of lantanum(Ⅲ) has been studied by adsorptive stripping voltammetry methods using an alizarin S as complexing agent and carbon paste electrode as working electrode. The electrode was made from mixed of carbon powder and paraffin in micropipette tip with diameter of 4 ram. This method consists of two steps. The first step is the formation and adsorptive accumulation of metal ion with chelator at the electrode surface. The second step is stripping the complex from the electrode surface into the solution. The stripping step generates current which is recorded as voltammogram. The optimum conditions of instrumental parameter obtained were accumulation potential of 600 mV, accumulation time of 120 seconds, and pH of solution of 5.5. In this research, the limit detection obtained was 2.3348 × 10^-12 M (3.24× 10^-11μg/L) with sensitivity of 16.52 (nA/10u M) and the precision of standard solution of La3+ with concentration of 2 × 10^-12 M, 4× 10^-12 M, 6 × 10^-12 M, 8 × 10^-12 M, and 10 × 10^-12M were 3.50%, 9.88%, 7.19%, 7.48% and 1.85% respectively. The linierity of this method is very good with correlation coefficient is 0.9780. Recovery percentage from La3+ with concentration of 6× 10^-12 M and 10 × 10^-12 M are 108.84% and 91.51%, respectively.展开更多
A new catalytic voltammetric method for the determination of anthraqunone medi-cines at a carbon paste electrode (CPE) was described for the first time. The mechanism of the catalytic reaction was investigated by usin...A new catalytic voltammetric method for the determination of anthraqunone medi-cines at a carbon paste electrode (CPE) was described for the first time. The mechanism of the catalytic reaction was investigated by using linear sweep voltammetry, cyclic voltammetry, con-stant potential electrolysis and so on. The experiment results indicate that aloe-emodin was effi-ciently accumulated at a CPE by adsorption. In the following potential scan, aloe-emodin was reduced to homologous anthrahydroquinone compound, then the compound was immediately oxidized to aloe-emodin by the dissolved oxygen, and the aloe-emodin was again reduced at the CPE. As a result, a cyclic catalytic reaction was established. But a reversible redox reaction of aloe-emodin can only be observed at a mercury electrode, no catalytic reaction occurs there. A sensitive catalytic voltammetric peak of aloe-emodin was obtained at about ?0.60 V (vs. SCE) in 0.56 mol/L NH3-NH4Cl buffer (pH 8.9). The proposed method was applied to the determination of aloe-emodin in the Radix Rhei with satisfactory results. The determination results were in good agreement with reference values obtained by the HPLC. The adsorptive catalytic voltammetry for the determination of organic compound at CPE, chemically modified electrode and other solid electrodes could be significant in the studies on pharmacology, pharmacodynamics, toxicity of medicine, clinical medicine and biochemistry.展开更多
A highly selective and rapid anodic adsorptive voltammetric method was developed for the (determination) of ultra trace amount of ofloxacin at a carbon paste electrode(CPE). The ofloxacin adsorbed on the surface o...A highly selective and rapid anodic adsorptive voltammetric method was developed for the (determination) of ultra trace amount of ofloxacin at a carbon paste electrode(CPE). The ofloxacin adsorbed on the surface of the CPE in a 0.096 mol/L KHP-NaOH buffer solution(pH=5.6) could produce one oxidation peak at 0.92 V(vs.SCE) when scanning was performed from 0.4 to 1.4 V. The relationship between the peak current and the ofloxacin concentration was linear in the ranges of 5.5×10-9~5.5×10-8 mol/L(75 s accumulation) and 3.3×10-8~3.3×10-7 mol/L(30 s accumulation). The correlation coefficients were 0.996 and 0.998, respectively. Its detection limit was 9.0×10-10 mol/L(S/N=3) for 150 s accumulation. The (electrode) reaction mechanism of ofloxacin was investigated. The proposed method was applied to analyze trace ofloxacin in urine samples. The result was in good agreement with that obtained by spectrophotometry (determination).展开更多
文摘A new sensitive adsorptive voltammetric method was described for the determination of zirconium at a carbon paste electrode (CPE) in the presence of alizarin complexone (ALC). Optimal analytical conditions are: 1.0?0-6 or 5.0?0-7 mol/L ALC, 0. 20 mol/L HAC-NaAc (pH 4.3), accumulation for 60 s at 0 V (vs. SCE), and linear scanning from 0 V to 1.0 V at 250 mV/s. The peak potential of the complex is at 0.81 V. By using a model JP-303 polarographic analyzer, 2.0?0-10 mol/L (S/N=3) zirconium can be detected with a 90 s accumulation, when the 2nd-order derivative linear sweep technique is used, and the linear range is 6.0?0-10-2.0?0-8 mol/L (5.0?0-7 mol/L ALC) and 2.0?0-8-2.0?0-7 mol/L (1.0?0-6 mol/L ALC), respectively. The developed method was applied to the determination of trace zirconium in the ore samples with satisfactory results.
文摘A sensitive method is described for the determination of trace antimony based on the antimony-bromopyrogallol red (BPR) adsorption at a carbon paste electrode (CPE). Three steps were involved in the overall analysis: preconcentration,reduction and stripping. Optimal conditions were found to be an electrode containing 25% paraffin oil and 75% high purity graphite powder as working electrode;a 0.10 mol/L HCl solution containing 40 μmol/L BPR as accumulation medium;a 0.20 mol/L HCl solution as reduction and stripping electrolyte;accumulation time,150 s;reduction potential and time,-0.50 V,60 s;scan range from -0.50 to 0.20 V. Interferences by other ions were studied as well. The detection limit was found to be 0.5 nmol/L for 150 s preconcentration. The linear range was from 1.0 nmol/L to 0.50 μmol/L. Application of the proposed method to the determination of antimony in water and human hair samples gave good results.
文摘This study presents the elaboration of a simple and cheap electrode made by carbon paste introduced into a cavity of electrode body, and used for the lead traces determination in tap water. A potentiostatic pre-electrolysis at constant voltage enables the reduction of the lead (Pb2+) and the accumulation of the metallic lead at and into the carbon paste;the reoxidation of the Pb (Linear sweep voltammetry) leads to the anodic striping peak. The effect of the main operating parameters on the shape of the peak and the magnitude of the current was examined and their optimal values were determined. Then calibration was achieved and the method was successfully applied (using all the optimized parameters) to the determination of lead in water, with a detection limit of 0.138 μg·L-1. Compared to other methods (ICP-AES for example), the proposed method offers a satisfactory detection limit of the Pb2+ (0.138 μg·L-1) because of the important specific area of the carbon paste electrode, for a significantly lower cost. Besides, there is no observed loss in the electrode answer in terms of peak current, which means that there is no any irreversible steps nor deactivation of the electrode, even after ten successive measurements;only reduction of the lead followed by the deposit oxidation was observed at the electrode.
文摘A novel method was described for the determination of ultra trace amount of scandium based on the cathodic adsorptive voltammetry of the mix-polynuclear complex of scandium-calcium-alizarin red S at a carbon paste electrode (CPE). The 2nd-order derivative linear scan voltammograms of the adsorbed complex were recorded by model JP-303 polarographic analyzer from 0.0 to -1.0 V (vs. SCE). The experimental conditions of the working procedure were optimized. The results show that the complex can be adsorbed on the surface of the CPE, yielding one peak at -0.61 V, corresponding to the reduction of the alizarin red S in the mix-polynuclear complex at the electrode. The detection limit of Sc^(3+) is 1.0×10^(-10) mol·L^(-1) for 3 min of accumulation time. The procedure was successfully applied to the determination of trace amount of scandium in the sample ores.
文摘A simple method for anodic stripping voltammetric determination of nitrite using carbon paste electrode modified with biomolecular chitosan, is described. In this method, the electrode is activated electrochemically by scanning 5 replicates over the potential range from +500 to +1400 mV immersing in 0.5 M HCl solution. Following this step, the nitrite sample containing 0.1 M KCl is preconcentrated on the activated electrode at +500 mV for 30 s. The deposited anions are then oxidized by different modes of sweep in the oxidation direction. Chemical and electrical parameters affecting the voltammetric measurements are optimized. The peak current is linear proportional to the NO2- concentration within the range 0.41 - 4.1 μg/ml, with detection limit 0.187 μg/m using differential pulse mode. The relative standard deviation is 0.285% for 2.46 μg/ml (five replicates). No interference is observed due to oxygen dissolved in the sample so that nitrogen purging is not needed in this case. The result obtained by the modified electrode is more accurate and selective than the unmodified electrode.
基金the Project of Science and Technology Fund of Hengyang City (Grant No. 2007KJ001)the Project of Scientific Research of Hengyang Normal University (Grant No. 07A19)+1 种基金the Key Project of Chinese Ministry of Education (Grant No. 206104)the Multidiscipline Scientific Research Foundation of Xiangtan Univer-sity (Grant No. 05IND08)
文摘A carbon paste electrode modified with multi-walled carbon nanotubes (MWCNT) was prepared and the determination of ultra trace amount of zirconium based on the anodic adsorptive voltammetry of the zirconium-calcium-alizarin red S mix-polynuclear complex is described in this paper for the first time. The results showed that the sensitivity and the selectivity of the method are excellent. The second de-rivative linear scan voltammograms of the complex were recorded by polarographic analyzer from 200 to 1200 mV (vs. SCE) and it was found that the complex can be adsorbed on the surface of the electrode, yielding a peak at about 840 mV, corresponding to the oxidation of ARS in the complex. The peak cur-rent increases linearly with Zr (IV) concentration in the range of 6.0×10-12―6.0×10-11 mol·L-1 (accumu-lation time 120 s), 6.0×10-11―2.0×10-9 mol·L-1 (accumulation time 90 s) and 2.0×10-9―1.0×10-7 mol·L-1 (accumulation time 60 s) and the detection limit (S/N = 3) is 2.0×10-12 mol·L-1 (accumulation time 180 s). The procedure has been successfully applied to the determination of zirconium in the ore samples.
基金Project supported by the National Natural Science Foundation of China (No. 20475043).
文摘Voltammetry using solid electrodes usually suffers from the contamination due to the deposition of the redox products of analytes on the electrode surface. The contamination has resulted in poor reproducibility and overelaborate operation procedures. The use of the chemical catalysis of oxidant on the reduction product of analyte not only can eliminate the contamination of analyte to solid electrodes but also can improve the faradaic response of analyte. This work introduced both the catalysis of oxidant K2S2O8 and the enhancement of surfactant Triton X-100 on the faraday response of amiodarone into an adsorptive stripping voltammetry at a carbon paste electrode for the determination of amiodarone. The method exhibits high sensitivity, good reproducibility and simple operation procedure. In 0.2 mol·L^-1 HOAc-NaOAc buffer (pH=5.3) containing 2.2×10^-2 mol·L^-1 K2S2O8 and 0.002% Triton X-100, the 2.5th-order derivative stripping peak current of the catalytic wave at 0.3 V (vs. Ag/AgCl) is rectilinear to amiodarone concentration in the range of 2.0×10^-10-2.3×10^-8 mol·L^-1 with a detection limit of 1.5×10^-10 mol·L^-1 after accumulation at 0 V for 30 s.
文摘Ultra trace determination of lantanum(Ⅲ) has been studied by adsorptive stripping voltammetry methods using an alizarin S as complexing agent and carbon paste electrode as working electrode. The electrode was made from mixed of carbon powder and paraffin in micropipette tip with diameter of 4 ram. This method consists of two steps. The first step is the formation and adsorptive accumulation of metal ion with chelator at the electrode surface. The second step is stripping the complex from the electrode surface into the solution. The stripping step generates current which is recorded as voltammogram. The optimum conditions of instrumental parameter obtained were accumulation potential of 600 mV, accumulation time of 120 seconds, and pH of solution of 5.5. In this research, the limit detection obtained was 2.3348 × 10^-12 M (3.24× 10^-11μg/L) with sensitivity of 16.52 (nA/10u M) and the precision of standard solution of La3+ with concentration of 2 × 10^-12 M, 4× 10^-12 M, 6 × 10^-12 M, 8 × 10^-12 M, and 10 × 10^-12M were 3.50%, 9.88%, 7.19%, 7.48% and 1.85% respectively. The linierity of this method is very good with correlation coefficient is 0.9780. Recovery percentage from La3+ with concentration of 6× 10^-12 M and 10 × 10^-12 M are 108.84% and 91.51%, respectively.
基金supported by the Scientific Research Funds of State Key Laboratory of Electroanalytical Chemistry of Changchun Institute of Applied Chemistry,Chinese Academy of Sciences.
文摘A new catalytic voltammetric method for the determination of anthraqunone medi-cines at a carbon paste electrode (CPE) was described for the first time. The mechanism of the catalytic reaction was investigated by using linear sweep voltammetry, cyclic voltammetry, con-stant potential electrolysis and so on. The experiment results indicate that aloe-emodin was effi-ciently accumulated at a CPE by adsorption. In the following potential scan, aloe-emodin was reduced to homologous anthrahydroquinone compound, then the compound was immediately oxidized to aloe-emodin by the dissolved oxygen, and the aloe-emodin was again reduced at the CPE. As a result, a cyclic catalytic reaction was established. But a reversible redox reaction of aloe-emodin can only be observed at a mercury electrode, no catalytic reaction occurs there. A sensitive catalytic voltammetric peak of aloe-emodin was obtained at about ?0.60 V (vs. SCE) in 0.56 mol/L NH3-NH4Cl buffer (pH 8.9). The proposed method was applied to the determination of aloe-emodin in the Radix Rhei with satisfactory results. The determination results were in good agreement with reference values obtained by the HPLC. The adsorptive catalytic voltammetry for the determination of organic compound at CPE, chemically modified electrode and other solid electrodes could be significant in the studies on pharmacology, pharmacodynamics, toxicity of medicine, clinical medicine and biochemistry.
文摘A highly selective and rapid anodic adsorptive voltammetric method was developed for the (determination) of ultra trace amount of ofloxacin at a carbon paste electrode(CPE). The ofloxacin adsorbed on the surface of the CPE in a 0.096 mol/L KHP-NaOH buffer solution(pH=5.6) could produce one oxidation peak at 0.92 V(vs.SCE) when scanning was performed from 0.4 to 1.4 V. The relationship between the peak current and the ofloxacin concentration was linear in the ranges of 5.5×10-9~5.5×10-8 mol/L(75 s accumulation) and 3.3×10-8~3.3×10-7 mol/L(30 s accumulation). The correlation coefficients were 0.996 and 0.998, respectively. Its detection limit was 9.0×10-10 mol/L(S/N=3) for 150 s accumulation. The (electrode) reaction mechanism of ofloxacin was investigated. The proposed method was applied to analyze trace ofloxacin in urine samples. The result was in good agreement with that obtained by spectrophotometry (determination).