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1.
A fast adsorptive stripping voltammetric procedure for simultaneous determination of Ni(II) and Co(II) in the presence of nioxime as a complexing agent at an in situ plated lead film electrode was described. The time of determination of these ions was shortened due to the application of gold as a substrate for lead film. At gold substrate lead film formation and accumulation of Ni(II) and Co(II) complexes with nioxime proceeds simultaneously. To obtain a stable signals for both ions a simple procedure of activation of the electrode was proposed. Calibration graphs for an accumulation time of 20 s were linear from 5×10?9 to 1×10?7 mol L?1 and from 5×10?10 to 1×10?8 mol L?1 for Ni(II) and Co(II), respectively. The procedure with the application of a lead film electrode on a gold substrate was validated in the course of Ni(II) and Co(II) determination in certified reference materials.  相似文献   

2.
For the first time an in situ plated bismuth film electrode has been applied to catalytic adsorptive stripping voltammetry of cobalt in the presence of nitrite. At optimised conditions bismuth film was plated before each measurement for 30 s at ?1.0 V from a sample solution with the added supporting electrolyte and Bi(III) in the form of its complex with tartrate. The calibration graph for Co(II) for an accumulation time of 120 s was linear from 5×10?10 to 1×10?8 mol L?1. The detection limit was 1.1×10?10 mol L?1. The proposed procedure was applied for Co(II) determination in certified water reference material.  相似文献   

3.
An adsorptive stripping voltammetric procedure for the determination of folic acid at an in situ plated lead film electrode was described. Formation of lead film on a glassy carbon substrate and accumulation of folic acid was performed simultaneously from an acetate buffer solution of pH 5.6 at the potential ?0.88 V. The measurements were carried out from aerated solutions. The calibration graph for an accumulation time of 300 s was linear from 2×10?9 to 5×10?8 mol L?1. The detection limit was 7×10?10 mol L?1, the relative standard deviation for 2×10?8 mol L?1 of folic acid was 3.9%. The proposed procedure was applied to folic acid determinations in pharmaceutical preparations.  相似文献   

4.
《Electroanalysis》2006,18(8):773-778
A sensitive and selective method for the determination of Pb(II) with a zirconium phosphated silica gel (SiZrPH) modified carbon paste electrode has been developed. The measurements were carried out in three steps including an open circuit accumulation following by electrolysis of accumulated Pb(II) at the modified carbon paste electrode and differential pulse voltammetric determination. The analytical performance was evaluated with respect to the carbon paste composition, pH of solution at the accumulation step, pH and concentration of supporting electrolyte, electrolysis potential, accumulation time and electrolysis time. Two linear calibration graphs were obtained in the concentration ranges 2.5×10?9 mol L?1–5.0×10?8 mol L?1 and 5.0×10?8 mol L?1–5.0×10?6 mol L?1 with an accumulation time of 120 s. The detection limit was found to be 3.5×10?10 mol L?1. The effects of potential interfering ions were studied, and it was found that the proposed procedure is free from interferences of common interfering ions such as tin, thallium and etc. The developed method was applied to Pb(II) determination in a wastewater sample.  相似文献   

5.
《Electroanalysis》2006,18(1):70-76
A lead‐copper film electrode was proposed for Co(II) determination by catalytic adsorptive stripping voltammetry. The electrode was plated in situ and hence the exchange of a solution after plating step was not required. At optimized conditions the calibration graph for Co(II) was linear from 5×10?10 to 2×10?8 mol L?1 for accumulation time of 15 s. The relative standard deviation for Co(II) determination at concentration 5×10?9 mol L?1 was 4.1%. The detection limits for Co(II) were 1.2×10?10 and 1.0×10?11 mol L?1 for an accumulation time of 15 and 180 s, respectively. The method was applied to Co(II) determination in certified reference material and other water samples.  相似文献   

6.
A sensor based in a graphite–polyurethane composite electrode modified with the mesoporous nanostructured silica with hexagonal array of pores called Santa Barbara Amorphous type material (SBA‐15) containing nickel was built. The presence of Ni, incorporated during the synthesis of SBA‐15, resulted in an increase in sensitivity when compared to the other electrodes based on the unmodified SBA‐15. A procedure was proposed for the determination of Cu2+ in ethanol biofuel by square wave stripping voltammetry with linear response in concentration levels of 1.0×10?8 and 1.0×10?7 mol L?1, resulting in a limit of detection of 1.83×10?10 mol L?1 and precision (RSD) of 2.09 %.  相似文献   

7.
This paper reports the use of an adsorptive voltammetric technique for Pb(II) determination using cupferron as a selective complexing agent. After accumulation of the complex onto a hanging mercury drop electrode, the electrode potential was scanned with differential pulse modulation and the reduction current of lead was observed at about??0.5?V. Under optimum conditions (5?×?10?4?mol?L?1 cupferron concentration, 0.1?mol?L?1 acetate buffer (pH 5.5), adsorption at??50?mV for 30?s) the detection limit was 5.1?×?10?10?mol?L?1. The relative standard deviation of five measurements for low lead concentration was 3.1%. The accuracy of the method was tested by analysing certified reference material (SPS-WW1 Waste Water). Finally, the method was successfully applied to the determination of Pb(II) in river water samples without any pretreatments.  相似文献   

8.
A multi-walled carbon nanotubes (MWNTs) modified glassy carbon electrode (MWNT-GCE) was used to study the electrochemical behaviour of1-hydroxypyrene (1-OHP) and applied to its determination. The results showed that the modified electrode had a strong adsorptive ability to 1-OHP and enhances its electrochemical signal. By square wave voltammetry, the linear relationship of 1-OHP was 6?×?10?9???8?×?10?7?mol?L?1 with a linear correlation coefficient of 0.996, and the detection limit was 1?×?10?10?mol?L?1. Compared with other published methods, this newly proposed method possesses many advantages such as very low detection limit, fast response, low cost and simplicity. And this method was applied successfully in the determination of 1‐OHP in real human urine samples.  相似文献   

9.
We report a simple and sensitive voltammetric sensor for the determination of chlorpromazine (CPZ) based on Ni?Al layered double hydroxide (NiAlLDH) modified glassy carbon electrode (GCE). NiAlLDH was simply electrodeposited on GCE surface in a very short time. The response linear range was 1×10?3–1×10?9 mol L?1, with a detection limit of 1×10?9 mol L?1. The NiAlLDH film showed well defined and well separate peaks for dopamine, ascorbic acid, uric acid and CPZ in the same solution. The proposed electrode was used to measure the active pharmaceutical ingredient of CPZ tablet as a real sample.  相似文献   

10.
This article the first reports on a fabrication and application of an electrochemical three electrode micro‐set containing: in situ plated lead film on carbon fiber working microelectrode, Ag/AgCl reference electrode and a platinum wire counter electrode placed in one casing for simultaneous Ni(II) and Co(II) traces determination by square wave adsorptive stripping voltammetry (SW AdSV). Ni(II) and Co(II) in forms of their complexes with nioxime were accumulated on the lead film plated on a carbon fibers microelectrode during standard procedure of measurement. Thanks to the fact that measurements were performed in micro‐vessel of a volume of 200 μl small amounts of reagents were used to prepare samples for measurements. In addition, because of the use of microelectrode, sample solutions were not mixed during accumulation step of measurements. This fact creates the possibility of conducting fields analysis. The experimental parameters (composition of the supporting electrolyte, potential and time of accumulation) and possible interference effects were investigated. The linear calibration graphs for Ni(II) and Co(II) were in the range from 2×10?9 to 1×10?7 mol L?1 and from 2×10?10 to 1×10?8 mol L?1 for Ni(II) and Co(II), respectively. The correctness of the proposed method was checked by determining Ni(II) and Co(II) in the certified reference material (SPS‐SW1) with satisfactory results.  相似文献   

11.
A new voltammetric procedure for the simultaneous determination of dopamine (DA) and paracetamol (PA) using boron doped diamond electrode modified with Nafion and lead films (PbF/Nafion/BDDE) was investigated. The use of this electrode resolved the overlapped voltammetric waves of DA and PA into well‐defined peaks with peak to peak separation of about 320 mV. Under the optimized experimental conditions in differential pulse voltammetric technique, DA and PA gave a linear response over the ranges 2.0×10?7–1.0×10?4 mol L?1*(R2=0.9996) and 5.0×10?7–1.0×10?3 mol L?1 (R2=0.9979), respectively. The detection limits were found to be 5.4×10?8 mol L?1 for DA and 1.4×10?7 mol L?1 for PA. They are lower, comparable or in some cases a little bit higher than those obtained using other electrochemical sensors. However, the proposed procedure of the sensor preparation is much simpler than procedures described in the literature with a lower detection limit. The proposed procedure was successfully applied to the determination of PA in some commercial pharmaceuticals as well as to the simultaneous determination of DA and PA in human urine, whole blood and serum samples directly without any separation steps.  相似文献   

12.
A new composite electrode is described for anodic stripping voltammetry determination of Pb(II) at trace level in aqueous solution. The electrode is based on the use of multiwalled carbon nanotubes and Amberlite IR-120. The anodic stripping voltammograms depend, to a large extent, on the composition of the modified electrode and the preconcentration conditions. Under optimum conditions, the anodic peak current at around ?0.57 V is linearly related to the concentration of Pb(II) in the range from 9.6?×?10?8 to 1.7?×?10?6 mol L?1 (R?=?0.998). The detection limit is 2.1?×?10?8 mol L?1, and the relative standard deviation (RSD) at 0.24?×?10?6 mol L?1 is 1.7% (n?=?6). The modified electrode was applied to the determination of Pb(II) using the standard addition method; the results showed average relative recoveries of 95% for the samples analysed.
Figure
A new composite electrode is described for anodic stripping voltammetry determination of Pb(II) at trace level in aqueous solution. The electrode is based on the use of MWCNT and Amberlite IR-120. The method showed a good linearity for 9.6?×?10?8 - 1.7?×?10?6 mol L?1 and detection limit of 2.1?×?10?8 mol L?1.  相似文献   

13.
Acibenzolar‐S‐methyl (ASM) is a novel fungicide applied for crop protection. A renewable silver amalgam film electrode was used for the determination of ASM in pH 3.4 Britton? Robinson buffer using square wave adsorptive stripping voltammetry (SW AdSV). The parameters of the method were optimized. The electroanalytical procedure made possible to determine ASM in the concentration range of 5×10?8–3×10?7 mol L?1 (LOD=4.86×10?9, LOQ=1.62×10?8 mol L?1). The effect of common interfering pesticides and heavy metal ions was checked. The validated method was applied in ASM determination in spiked water samples.  相似文献   

14.
The paper presents the first report on application of a “hybrid” lead film electrode for the adsorptive stripping voltammetric determination of Ni(II) in the presence of nioxime as a complexing agent. The strategy to create a “hybrid” electrode is based on the combination of ex situ and in situ plating methods and the use of a reversibly deposited mediator metal (Zn) for the lead film formation. The surface morphology of a new sensor was characterized by atomic force microscopy. The detection limit for Ni(II) obtained at 120 s of accumulation time was 3.9×10?11 mol L?1. The proposed method was validated for the determination of nickel in water certified reference materials with good results.  相似文献   

15.
An adsorptive stripping voltammetric procedure for the determination of cobalt in a complex matrices at an in situ plated lead film electrode was described. The procedure exploits the enhancement effect of a cobalt peak observed in the system Co(II)–nioxime–piperazine‐1,4‐bis(2‐ethanesulfonic acid)–cetyltrimethylammonium bromide. The calibration graph was linear from 5×10?10 to 2×10?8 mol L?1 and from 1×10?10 to 1×10?9 mol L?1 for the accumulation times 120 and 600 s, respectively. The detection limit (based on the 3 σ criterion) for Co(II) following accumulation time of 600 s was 1.1×10?11 mol L?1. The interference of high concentrations of foreign ions and surfactants was studied.  相似文献   

16.
Several problems for the direct electrochemical oxidation of reduced glutathione (GSH) challenge the usage of electroanalytical techniques for its determination. In this work, the electrochemical oxidation of GSH catalyzed by gold nanoparticles electrodeposited on Nafion modified carbon paste electrode in 0.04?mol?L?1 universal buffer solution (pH?7.4) is proved successful. The effect of various experimental parameters including pH, scan rate and stability on the voltammetric response of GSH was investigated. At the optimum conditions, the concentration of GSH was determined using differential pulse voltammetry (DPV) in two concentration ranges: 0.1?×?10?7 to 1.6?×?10?5?mol?L?1 and 2.0?×?10?5 to 2.0?×?10?4?mol?L?1 with correlation coefficients 0.9988, 0.9949 and the limit of detections (LOD) are 3.9?×?10?9?mol?L?1 and 8.2?×?10?8?mol?L?1, respectively, which confirmed the sensitivity of the electrode. The high sensitivity, wide linear range, good stability and reproducibility, and the minimal surface fouling make this modified electrode useful for the determination of spiked GSH in urine samples and in tablet with excellent recovery results obtained.  相似文献   

17.
In this article a solid lead electrode (PbE) was utilized for the first time for determination of organic substances by means of adsorptive stripping voltammetry. A new procedure of simultaneous determination of rutin and folic acid was developed. Two well shaped and well separated reduction signals of rutin and folic acid were obtained with the use of PbE. The optimization of analytical procedure was presented. The calibration graphs for rutin and folic acid for an accumulation time of 120 s were linear in the ranges from 2×10?9 to 1×10?7 mol L?1 and from 2×10?9 to 5×10?8 mol L?1, respectively. The obtained detection limits for rutin and folic acid determination following accumulation time of 120 s were 7.9×10?10 and 8.4×10?10 mol L?1. Potential interference effects were investigated. The proposed procedure was used for analysis of pharmaceutical preparations with satisfactory results showing practical applications. The analytical parameters of the proposed procedure were compared with other voltammetric procedures of mentioned substances determination.  相似文献   

18.
In this paper, a novel poly(aminosulfonic acid) modified glassy carbon electrode (PASA/GCE) for the determination of Sudan II was fabricated through electrochemical polymerizat ion. The electrochemical behavior of Sudan II at the modified electrode was studied by cyclic voltammetry. Results show that the modified electrode exhibits excellent electrocatalytic activity toward the electrochemical redox reaction of Sudan II. Under optimal experimental conditions, the oxidation peak current is linearly proportional to the concentration of Sudan II in the ranges of 4.0 × 10?8 to 1.0 × 10?6 mol L?1 and 1.0 × 10?6 to 1.2 × 10?5 mol L?1. The linear regression equations are i pa(A) = 2.87c + 3.74 × 10?6, r = 0.9977 and i pa(A) = 0.78c + 6.11 × 10?6, r = 0.9982, respectively, and the detection limit is 4.0 × 10?9 mol L?1. The novel method shows good recovery, reproducibility and sensitivity for the voltammetric determination of Sudan II in food samples.  相似文献   

19.
A novel kind of carbon paste electrode (CPE) was prepared by mixing graphite powder, liquid paraffin and the ionic liquid 1-ethyl-3-methylimidazolium ethylsulfate. The resulting electrode was used for the simultaneous determination of guanosine and adenosine by differential pulse voltammetry. Compared to a conventional CPE, the oxidation peak currents are largely increased, and the oxidation peak potentials are negatively shifted. The electrochemical responses to guanosine and adenosine were investigated. Under optimized conditions, the calibration curves are linear in the concentration range from 1.0?×?10-6?mol?L-1 to 1.6?×?10-4?mol?L-1 for guanosine, and from 1.0?×?10-6?mol?L-1 to 2.7?×?10-4?mol?L-1 for adenosine at pH 3.5. Substances potentially interfering in the biological matrix do no interfere. The method was successfully applied to detect adenosine and guanosine in human urine without sample treatments.
Figure
Cyclic voltammograms on CPE (a) and CILE (b) for 1.0?×?10-4?mol?L-1 adenosine and 1.0?×?10-4?mol?L-1guanosine in a pH 3.5 B-R buffer solution at the scan rate of 100?mV?s-1. Inset was the typical differential pulse voltammograms of 1.0?×?10-4?mol?L-1 adenosine and 1.0?×?10-4?mol?L-1?L guanosine on CILE  相似文献   

20.
《Analytical letters》2012,45(13):2026-2040
Abstract

The potentiometric response characteristics of a new copper(II) ion-selective PVC membrane electrode based on erythromycin ethyl succinate (EES) as ionophore were investigated. The electrode exhibited a Nernstian response to Cu2+ ions over the activity range of 1.5 × 10?2 to 2.0 × 10?6 mol L?1 with a limit of detection of 6.3 × 10?7 mol L?1. Stable potentials were obtained in the pH range of 5.5–6.5. The potentiometric selectivity coefficients were calculated by using fixed interference method and revealed no important interferences except for Ag+. This electrode was successfully applied as an indicator electrode in determination of copper ions in real water samples.  相似文献   

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