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1.
A new chemically modified carbon paste electrode was constructed and used for rapid, simple, accurate, selective and highly sensitive simultaneous determination of cadmium, copper and mercury using square wave anodic stripping voltammetry (SWASV). The carbon paste electrode was modified by N,N′-bis(3-(2-thenylidenimino)propyl)piperazine coated silica nanoparticles. Compared with carbon paste electrode, the stripping peak currents had a significant increase at the modified electrode. Under the optimized conditions (deposition potential, −1.100 V vs. Ag/AgCl; deposition time, 60 s; resting time, 10 s; SW frequency, 25 Hz; pulse amplitude, 0.15 V; dc voltage step height, 4.4 mV), the detection limit was 0.3, 0.1 and 0.05 ng mL−1 for the determination of Cd2+, Cu2+ and Hg2+, respectively. The complexation reaction of the ligand with several metal cations in methanol was studied and the stability constants of the complexes were obtained. The effects of different cations and anions on the simultaneous determination of metal ions were studied and it was found that the electrode is highly selective for the simultaneous determination of Cd2+, Cu2+ and Hg2+. Furthermore, the present method was applied to the determination of Cd2+, Cu2+ and Hg2+ in water and some foodstuff samples.  相似文献   

2.
The use of selective pre-concentration and differential pulse anodic stripping voltammetry (DPASV) using a carbon paste electrode modified (CPEM) with spinel-type manganese oxide has been proposed for the determination of lithium ions content in natural waters. The new procedure is based on the effective pre-concentration of lithium ions on the electrode surface containing spinel-type Mn(IV) oxide with the reduction of Mn(IV) to Mn(III) and consequently the lithium ions intercalation (insertion) into the spinel structure. The best DPASV response was reached for an electrode composition of 25% (m/m) spinel-type MnO2 in the paste, 0.1 mol l−1 tris(hydroxymethyl)aminomethane (TRIS) buffer solution of pH 8.3, scan rate of 5 mV s−1, accumulation potential of 0.3 V versus saturated calomel reference electrode (SCE), pre-concentration time of 30 s and potential pulse amplitude of 50 mV. In these experimental conditions, the proposed methodology responds to lithium ions in the concentration range of 2.8×10−6 to 2.0×10−3 mol l−1 with a detection limit of 5.6×10−7 mol l−1. The determination of the lithium ions content in different samples of natural waters samples using the proposed methodology and atomic absorption spectrophotometry are in agreement at the 95% confidence level and within an acceptable range of error.  相似文献   

3.
The preparation of Hg(II)-modified multi walled carbon nanotube (MWCNT) by reaction of oxidized MWCNT with aqueous HgCl2 was carried out. The Hg(II)-modified multi walled carbon nanotube (Hg(II)/MWCNT) dispersed in Nafion solution was used to coat the polished graphite electrode surface. The Hg(II)/MWCNT modified graphite electrode was held at a cathodic potential (−1.0 V) to reduce the coordinated Hg(II) to Hg forming nanodroplets of Hg. The modified electrode was characterized by FESEM/EDAX which provided useful insights on the morphology of the electrode. The SEM images showed droplets of Hg in the size of around 260 nm uniformly distributed on the MWCNT. Differential pulse anodic stripping voltammetry (DPASV) and electrochemical impedance spectroscopy were used to study the Hg(II) binding with MWCNT. Differential pulse anodic stripping voltammetry of ppb levels of cadmium and lead using the modified electrode yielded well-defined peaks with low background current under a short deposition time. Detection limit of 0.94 and 1.8 ng L−1 were obtained following a 3 min deposition for Pb(II) and Cd(II), respectively. Various experimental parameters were characterized and optimized. High reproducibility was observed from the RSD values for 20 repetitive measurements of Pb(II) and Cd(II) (1.7 and 1.9%, respectively). The determination of Pb(II) and Cd(II) in tap water and Pb(II) in human hair samples was carried out. The above method of fabrication of Hg(II)/MWCNT modified graphite electrode clearly suggests a safe route for preparing Hg immobilized electrode for stripping analysis.  相似文献   

4.
The present work describes the development of a modified platinum electrode for stripping voltammetric determination of silver. The deposition of films based on electropolymerisation of the monomer thiophene was carried out by cycling the potential towards positive values between 0 and 1.6 V.The preconcentration process of silver ions was initiated on the surface of the modified electrode by complexing silver with polythiophene (PTH) when a negative potential (−0.5 V) was applied; then the reduced products was oxidized by means of differential pulse stripping voltammetry and the peak was observed at 0.17 V. Parameters such as pH, supporting electrolyte and number of electropolymerisation cycles were studied. A linear relation between current peak and concentration of Ag(I) was obtained in the range 0.07-1.0 mg L−1. The detection limit for Ag(I) was evaluated to be 0.06 mg L−1. The reproducibility was tested carrying out 11 measurements at different electrodes and the relative standard deviation was 1.5%. The interference of several metals was investigated and showed negligible effect on the electrode response.  相似文献   

5.
The study of a new type of working electrode - the renovated silver ring electrode (RSRE) - for lead ions detection via differential pulse anodic stripping voltammetry (DP ASV) without removal of oxygen is reported. The only four constituents of the RSRE: a specially constructed silver ring electrode, a silver sheet used as silver counter/quasi-reference electrode and a silicon O-ring, are fastened together in a polypropylene body. The renovation of this electrode is carried out through mechanical removal of solid contaminants and electrochemical activation in the electrolyte which fills the RSRE body. Excellent repeatability and reproducibility - also in organic samples solutions - were reached in a period of a few weeks through the renovation of the electrode surface before each measurement. The reduction and stripping of lead on silver electrode under the DP ASV conditions are underpotential deposition/dissolution phenomena. The RSRE is used for the determination of Pb ions in concentrations ranging from 1 × 10−9 to 1 × 10−7 M. The repeatability of DP ASV runs in synthetic solutions covering the entire concentration range is better than 2%. Obtained calibration curves are represented by a correlation coefficient of at least 0.999. The detection limit (LOD) for the time of electrodeposition equal to 60 s is 0.2 × 10−9 M. LOD for Pb2+ detection at the RSRE is similar to this reported for a rotating silver electrode in subtractive anodic stripping voltammetry (E. Kirowa-Eisner, et al., Anal. Chim. Acta, 385 (1999) 325). The analysis of Pb2+ in synthetic solutions with and without surfactants, certified reference materials and natural water samples have been performed.  相似文献   

6.
The efficacy of silver-deposited glassy carbon electrode for the determination of lead ions at the sub-nanomolar concentration ranges is investigated. The silver nanoparticles are electrodeposited on glassy carbon electrode using chronoamperometry and the electrode surface is characterized using SEM. Lead ions are detected in the region of underpotential deposition. The analysis is performed in square wave mode in the stripping voltammetry without the removal of oxygen. The detection limit of 10 pM has been obtained with a constant potential of −0.7 V during the electrodeposition step for a period of 50 s. The interference of surfactants in the detection of lead ions is also studied.  相似文献   

7.
A typical, reproducible, and rugged screen printed carbon electrode, modified with dual-ion imprinted beads, was fabricated employing the “surface grafting from” approach. For this, the acyl chloride functionalized magnetic nanoparticles were first immobilized and chemically attached with a typical functional monomer (but-2-enedioic acid bis-[(2-amino-ethyl)-amide]) on the electrode surface. This was subsequently subjected to the thermal polymerization in the presence of template ions (Ce(IV) and Gd(III)), cross-linker (ethylene glycol dimethacrylate), initiator (AIBN), and multiwalled carbon nanotubes. The modified sensor was used for the simultaneous analysis of both template ions in aqueous, blood serum, and waste-water samples, using differential pulse anodic stripping voltammetry which revealed two oxidation peaks for respective templates with resolution as much as 950 mV, without any cross reactivity, interferences and false-positives. The detection limits realized by the proposed sensor, under optimized conditions, were found to be as low as 0.07 ng mL−1 for Ce(IV) and 0.19 ng mL−1 for Gd(III) (S/N = 3) that could eventually be helpful for lanthanide estimation at stringent levels.  相似文献   

8.
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   

9.
Alireza Mohadesi 《Talanta》2007,71(2):615-619
A differential pulse anodic stripping voltammetric method was developed for the determination of Ag(I) at a 3-amino-2-mercapto quinazolin-4(3H)-one modified carbon paste electrode. The analysis procedure consisted of an open circuit accumulation step in stirred sample solution for 12 min. This was followed by medium exchange to a clean solution where the accumulated Ag(I) was reduced for 15 s in −0.6 V. Subsequently an anodic potential scan was effected from −0.2 to +0.2 V to obtain the voltammetric peak. The detection limit of silver(I) was 0.4 μg L−1 and R.S.D. for 10, 100 and 200 μg L−1 silver(I) were 2.4, 1.8 and 1.3%, respectively. The calibration curve was linear for 0.9-300 μg L−1 silver(I). Many coexisting ions had little or no effect on the determination of silver(I). The procedure was applied to determination of silver(I) in X-ray photographic films and natural waters. In X-ray photographic film samples, the results have compared to those obtained by atomic absorption spectroscopy.  相似文献   

10.
An in-situ antimony film screen-printed carbon electrode (in-situ SbSPCE) was successfully used for the determination of Cu(II) simultaneously with Cd(II) and Pb(II) ions, by means of differential pulse anodic stripping voltammetry (DPASV), in a certified reference groundwater sample with a very high reproducibility and good trueness. This electrode is proposed as a valuable alternative to in-situ bismuth film electrodes, since no competition between the electrodeposited copper and antimony for surface sites was noticed. In-situ SbSPCE was microscopically characterized and experimental parameters such as deposition potential, accumulation time and pH were optimized. The best voltammetric response for the simultaneous determination of Cd(II), Pb(II) and Cu(II) ions was achieved when deposition potential was −1.2 V, accumulation time 120 s and pH 4.5. The detection and quantification limits at levels of μg L−1 suggest that the in-situ SbSPCE could be fully suitable for the determination of Cd(II), Pb(II) and Cu(II) ions in natural samples.  相似文献   

11.
Three different electroanalytical techniques for the detection of manganese in marine sediments are evaluated. The anodic stripping voltammetry of manganese at an in situ bismuth-film-modified boron-doped diamond electrode and cathodic stripping voltammetry at a carbon paste electrode are shown to lack the required sensitivity and reproducibility whereas cathodic stripping voltammetry at a bare boron-doped diamond electrode is shown to be reliable and selective with a limit of detection, from applying a 60 s accumulation period of 7.4 × 10−7 M and a sensitivity of 0.24 A M−1. The method was used to evaluate the manganese content of marine sediments taken from Šibenik, Croatia.  相似文献   

12.
Yasri NG  Halabi AJ  Istamboulie G  Noguer T 《Talanta》2011,85(5):2528-2533
A new simple chronoamperometry methodology was developed for the ultrasensitive determination of lead ions using a PEDOT:PSS coated graphite carbon electrode. The polymer was directly coated on a graphite carbon electrode and characterized using simple cycle voltammetric measurements. The presence of lead ions induced a cathodic peak starting at −550 ± 10 mV vs. Ag/AgCl, and an anodic peak starting at −360 ± 10 mV vs. Ag/AgCl. Electroaccumulation of lead ions onto the PEDOT:PSS modified electrode was performed at −650 mV vs. Ag/AgCl for 30 s in a pH 2.2 hydrochloric acid solution. Chronoamperometry measurements were carried out at −350 mV vs. Ag/AgCl allowing the oxidation of accumulated lead. Using this method, lead ions were detected for concentrations ranging between 2.0 nmol L−1 and 0.1 μmol L−1 (R2 = 0.999). The detection limit was calculated to be 0.19 nmol L−1 and the quantification limit of 0.63 nmol L−1. The method was shown to be highly precise and sensitive, negligible interference was detected from other metal ions. The proposed method was successfully applied for the detection of lead ions in vegetables.  相似文献   

13.
A multi-wall carbon nanotube (MWNT) modified glassy carbon electrode (GCE) was described for the simultaneous determination of trace levels of cadmium and lead by anodic stripping voltammetry (ASV). In pH 4.5 NaAc-HAc buffer containing 0.02 mol/l KI, Cd2+ and Pb2+ first adsorb onto the surface of a MWNT film coated GCE and then reduce at −1.20 V. During the positive potential sweep, reduced cadmium and lead were oxidized, and two well-defined stripping peaks appeared at −0.88 and −0.62 V. Compared with a bare GCE, a MWNT film coated GCE greatly improves the sensitivity of determining cadmium and lead. Low concentration of I significantly enhances the stripping peak currents since it induces Cd2+ and Pb2+ to adsorb at the electrode surface. The striping peak currents change linearly with the concentration of Cd2+ from 2.5×10−8 to 1×10−5 mol/l and with that of Pb2+ from 2×10−8 to 1×10−5 mol/l. The lowest detectable concentrations of Cd2+ and Pb2+ are estimated to be 6×10−9 and 4×10−9 mol/l, respectively. The high sensitivity, selectivity, and stability of this MWNT film coated electrode demonstrated its practical application for a simple, rapid and economical determination of trace levels of Cd2+ and Pb2+ in water samples.  相似文献   

14.
M. Ghiaci  R.J. Kalbasi 《Talanta》2007,73(1):37-45
The main purpose of this study is to develop an inexpensive, simple, selective and especially highly selective modified mixed-oxide carbon paste electrode (CPE) for voltammetric determination of Pb(II). For the preliminary screening purpose, the catalyst was prepared by modification of SiO2-Al2O3 mixed-oxide and characterized by TG, CHN elemental analysis and FTIR spectroscopy. Using cyclic voltammetry the electroanalytical characteristics of the catalyst have been determined, and consequently the modified mixed-oxide carbon paste electrode was constructed and applied for determination of Pb(II). The electroanalytical procedure for determination of the Pb(II) comprises two steps: the chemical accumulation of the analyte under open-circuit conditions followed by the electrochemical detection of the preconcentrated species using differential pulse anodic stripping voltammetry. During the preconcentration step, Pb(II) was accumulated on the surface of the modifier by the formation of a complex with the nitrogen atoms of the pyridyl groups in the modifier. The peak currents increases linearly with Pb(II) concentration over the range of 2.0 × 10−9 to 5.2 × 10−5 mol L−1 (r2 = 0.9995).The detection limit (three times signal-to-noise) was found to be 1.07 × 10−9 mol L−1 Pb(II). The chemical and instrumental parameters have been optimized and the effect of the interferences has been determined. The Proposed method was used for determination of lead ion in the real samples.  相似文献   

15.
Yan Wang  Zhen-zhen Chen 《Talanta》2010,82(2):534-621
This report described the direct voltammetric detection of peroxynitrite (ONOO) at a novel cyanocobalamin modified glassy carbon electrode prepared by electropolymeriation method. The electrochemical behaviors of peroxynitrite at the modified electrode were studied by cyclic voltammetry. The results showed that this new electrochemical sensor exhibited an excellent electrocatalytic activity to oxidation of peroxynitrite. The mechanism of catalysis was discussed. Based on electrocatalytic oxidation of peroxynitrite at the poly(cyanocobalamin) modified electrode, peroxynitrite was sensitively detected by differential pulse voltammetry. Under optimum conditions, the anodic peak current was linear to concentration of peroxynitrite in the range of 2.0 × 10−6 to 3.0 × 10−4 mol L−1 with a detection limit of 1.0 × 10−7 mol L−1 (S/N of 3). The proposed method has been applied to determination of peroxynitrite in human serum with satisfactory results. This poly(cyanocobalamin) modified electrode showed high selectivity and sensitivity to peroxynitrite determination, which could be used in quantitative detection of peroxynitrite in vivo and in vitro.  相似文献   

16.
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   

17.
The present paper has focused on the potential application of the bifunctional polydopamine@Fe3O4 core–shell nanoparticles for development of a simple, stable and highly selective electrochemical method for metal ions monitoring in real samples. The electrochemical method is based on electrochemical preconcentration/reduction of metal ions onto a polydopamine@Fe3O4 modified magnetic glassy carbon electrode at −1.1 V (versus SCE) in 0.1 M pH 5.0 acetate solution containing Pb2+ and Cd2+ during 160 s, followed by subsequent anodic stripping. The proposed method has been demonstrated highly selective and sensitive detection of Pb2+ and Cd2+, with the calculated detection limits of 1.4 × 10−11 M and 9.2 × 10−11 M. Under the optimized conditions, the square wave anodic stripping voltammetry response of the modified electrode to Pb2+ (or Cd2+) shows a linear concentration range of 5.0–600 nM (or 20–590 nM) with a correlation coefficient of 0.997 (or 0.994). Further, the proposed method has been performed to successfully detect Pb2+ and Cd2+ in aqueous effluent.  相似文献   

18.
Graphene nanosheets, dispersed in Nafion (Nafion-G) solution, were used in combination with in situ plated bismuth film electrode for fabricating the enhanced electrochemical sensing platform to determine the lead (Pb2+) and cadmium (Cd2+) by differential pulse anodic stripping voltammetry (DPASV). The electrochemical properties of the composite film modified glassy carbon electrode were investigated. It is found that the prepared Nafion-G composite film not only exhibited improved sensitivity for the metal ion detections, but also alleviated the interferences due to the synergistic effect of graphene nanosheets and Nafion. The linear calibration curves ranged from 0.5 μg L−1 to 50 μg L−1 for Pb2+ and 1.5 μg L−1 to 30 μg L−1 for Cd2+, respectively. The detection limits (S/N = 3) were estimated to be around 0.02 μg L−1 for Pb2+ and Cd2+. The practical application of the proposed method was verified in the water sample determination.  相似文献   

19.
Yuan S  Chen W  Hu S 《Talanta》2004,64(4):922-928
An anthraquinone (AQ) improved Na-montmorillonite nanoparticles (nano-SWy-2) chemically modified electrode (CME) has been developed for the simultaneous determination of trace levels of cadmium (II) and lead (II) by differential pulse anodic stripping voltammetry (DPASV). This method is based on a non-electrolytic preconcentration via ion exchange model, followed by an accumulation period via the complex formation in the reduction stage at −1.2 V, and then by an anodic stripping process. The mechanism of this design was proposed and the analytical performance was evaluated with several variables. Under the optimized working conditions, the detection limit was 3 and 1 nM for Cd2+ and Pb2+, respectively. The calibration graphs were linear in the concentration ranges of 8×10−9 to 1×10−6 mol L−1 (Cd2+) and of 2×10−9 to 1×10−6 mol L−1 (Pb2+). Many inorganic species did not interfere with the assay significantly; the high sensitivity, selectivity, and stability of this nano-SWy-2-AQ CME were demonstrated. The applications for the detection of trace levels of Cd2+ and Pb2+ in milk powder and lake water samples indicate that it is an economical and potent method.  相似文献   

20.
Solid paraffin-based carbon paste electrodes modified with 2-aminothiazole organofunctionalized silica have been applied to the anodic stripping determination of copper ions in ethanol fuel samples without any sample treatment. The proposed method comprised four steps: (1) copper ions preconcentration at open circuit potential directly in the ethanol fuel sample; (2) exchange of the solution and immediate cathodic reduction of the absorbate at controlled potential; (3) differential pulse anodic stripping voltammetry; (4) electrochemical surface regeneration by applying a positive potential in acid media. Factors affecting the preconcentration, reduction and stripping steps were investigated and the optimum conditions were employed to develop the analytical procedure. Using a preconcentration time of 20 min and reduction time of 120 s at −0.3 V versus Ag/AgClsat a linear range from 7.5 × 10−8 to 2.5 × 10−6 mol L−1 with detection limit of 3.1 × 10−8 mol L−1 was obtained. Interference studies have shown a decrease in the interference effect according to the sequence: Ni > Zn > Cd > Pb > Fe. However, the interference effects of these ions have not forbidden the application of the proposed method. Recovery values between 98.8 and 102.3% were obtained for synthetic samples spiked with known amounts of Cu2+ and interfering metallic ions. The developed electrode was successfully applied to the determination of Cu2+ in commercial ethanol fuel samples. The results were compared to those obtained by flame atomic absorption spectroscopy by using the F-test and t-test. Neither F-value nor t-value have exceeded the critical values at 95% confidence level, confirming that there are no significant differences between the results obtained by both methods.  相似文献   

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