首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 31 毫秒
1.
《Analytical letters》2012,45(13):2045-2055
Abstract

A new method for determination of trace indium is proposed by the adsorption stripping voltammetry (ASV) using a Nafion‐modified glassy carbon electrode (NMGCE). This chemically modified electrode (CME) shows a better stability. A sensitive oxidation peak was observed, and the anodic peak potential is ca. ?0.548 V (vs. SCE). The influences of various experimental parameters on the current peak were completely studied. Under the optimized condition, the method has been applied to the determination of indium in water samples. There is a good linear relationship between the peak current (ip) and indium(III) concentration in the range of 1.0×10?9–1.0×10?7 mol/l, and the limit of detection is 7.5×10?10 mol/l.  相似文献   

2.
A method for the determination of nickel(II) by stripping voltammetry is described. The method is based on the adsorptive accumulation of nickel(II) calconcarboxylic acid complex onto a hanging mercury drop electrode (HMDE), followed by the reduction of the adsorbed complex using differential pulse voltammetry. The optimum operating conditions and parameters were found to be 0.05 M NH3/NH4Cl buffer (pH = 9.5) as the supporting electrolyte, a ligand concentration of 1 × 10?6 M, accumulation potential of ?0.5 V (vs. Ag/AgCl) and accumulation time of 60 s. At the optimized conditions, the peak current is proportional to the concentration of nickel in the range of 1.7 × 10?9 to 4.7 × 10?7 M (0.1–28 ng ml?1) with a detection limit of 0.05 ng ml?1. The relative standard deviation (n = 10) at nickel concentrations of 2, 10 and 15 ng ml?1 varies in the range 0.76 to 2.1%. Possible interferences by metal ions, which are of great significance in real matrices, have been studied. The method was successfully applied to the determination of nickel content in a chocolate sample.  相似文献   

3.
《Analytical letters》2012,45(14):2693-2707
Abstract

In the present work, an adsorptive cathodic stripping voltammetric method using a hanging mercury drop electrode (HMDE) was described in order to determine the ultra trace of lead ions with carbidopa in different real samples. The method is based on accumulation of lead metal ion on mercury electrode using carbidopa as a suitable complexing agent. The potential was scanned to the negative direction and the differential pulse stripping voltammograms were recorded. The instrumental and chemical parameters were optimized. The optimized conditions were obtained in pH of 8.4, carbidopa amount of 1.0×10?6 M, accumulation potential of 0. 0 V, accumulation time of 100 s, scan rate of 100 mV/s and pulse height of 50 mV. The relationship between the peak current versus concentration was linear over the range of 2.4×10?10–4.8×10?7 M. The limits of detection were 5.8×10?11 M and the relative standard deviation at 4.8×10?10, 2.1×10?8, and 2.4×10?7 M of lead ion were obtained 3.2, 2.9, and 2.7%, respectively (n=7).  相似文献   

4.
In this paper, a gold nanoparticle-modified indium tin oxide electrode (Au/ITO) was prepared without the use of any cross-linker or stabilizer reagent. The prepared Au/ITO was used as a new platform to achieve the direct electron transfer between Hb and the modified electrode. The proposed electrode exhibited a pair of well-defined redox peaks with a formal potential of ?0.073 V (vs. Ag/AgCl). The immobilized Hb showed excellent electrocatalytic activity toward H2O2 and the electrocatalytic current values were linear with the increasing concentration of H2O2 ranging from 1.0?×?10?6?M to 7.0?×?10?4?M. The detection limit was 2.0?×?10?7?M (S/N?=?3) and the Michaelis–Menten constant was calculated to be 0.2 mM. The proposed electrode also showed high selectivity, long-term stability, and good reproducibility.  相似文献   

5.
《Analytical letters》2012,45(7):1208-1224
Abstract

This paper describes development of a new analysis system for determination of lorazepam by a novel square wave voltammetry method to perform a very sensitive method. The method used for determination of lorazepam involves measuring the changes in admittance voltammogram of a gold ultramicroelectrode (in 0.05 M H3PO4 solution) caused by adsorption of the lorazepam on the electrode surface. Variation of admittance in the detection process is created by inhibition of oxidation reaction of the electrode surface, by adsorbed lorazepam. Furthermore, signal-to-noise ratio is significantly increased by application of discrete fast Fourier transform (FFT) method, background subtraction, and two-dimensional integration of the electrode response over a selected potential range and time window. Also in this work, some parameters such as SW frequency, eluent pH, and accumulation time were optimized. Calibration plots are given for solutions containing 10?6–10?11 M of lorazepam. The detection limit is calculated to be 6.0 × 10?12 M (~ 2 pg/ml). The relative standard deviation at concentration 3.0 × 10?8 M is 6.1% for 5 reported measurements.  相似文献   

6.
A novel enzyme-free electrochemical sensor for H2O2 was fabricated by modifying an indium tin oxide (ITO) support with (3-aminopropyl) trimethoxysilane to yield an interface for the assembly of colloidal gold. Gold nanoparticles (AuNPs) were then immobilized on the substrate via self-assembly. Atomic force microscopy showed the presence of a monolayer of well-dispersed AuNPs with an average size of ~4 nm. The electrochemical behavior of the resultant AuNP/ITO-modified electrode and its response to hydrogen peroxide were studied by cyclic voltammetry. This non-enzymatic and mediator-free electrode exhibits a linear response in the range from 3.0?×?10?5 M to 1.0?×?10?3 M (M?=?mol?·?L?1) with a correlation coefficient of 0.999. The limit of detection is as low as 10 nM (for S/N?=?3). The sensor is stable, gives well reproducible results, and is deemed to represent a promising tool for electrochemical sensing.
Figure
AuNPs/ITO modified electrode prepared by self-assembly method exhibit good electrocatalytic activity towards enzyme-free detection H2O2. The linear range of typical electrode is between 3.0?×?10?5 M and 1.0?×?10?3 M with a correlation coefficient of 0.999 and the limit detection is down to 1.0?×?10?8 M.  相似文献   

7.
《Analytical letters》2012,45(7):1128-1143
Abstract

The spectrophotometric behavior of uranium (VI) with L-3-(3, 4-dihydroxy phenyl) alanine (LDOPA) reagent revealed that the uranium can form a ML2 complex with LDOPA in solution. Thus a highly sensitive adsorptive stripping voltammetric protocol for measuring of trace uranium, in which the preconcentration was achieved by adsorption of the uranium-LDOPA complex at hanging mercury drop electrode (HMDE), is described. Optimal conditions were found to be a 0.02 M ammonium buffer (pH 9.5) containing 2.0 × 10?5 M (LDOPA), an accumulation potential of ? 0.1 V (versus Ag/AgCl) and an accumulation time of 120 sec.

The peak current and concentration of uranium accorded with linear relationship in the range of 0.5–300 ng ml?1. The relative standard deviation (at 10 ng ml?1) is 3.6% and the detection limit is 0.27 ng ml?1. The interference of some common ions was studied. Applicability to different real samples is illustrated. The attractive behavior of this reagent holds great promise for routine environmental and industrial monitoring of uranium.  相似文献   

8.
Differential pulse and cyclic voltammetry were applied for the oxidation of mixture of uric acid and ascorbic acid at the surface of carbon paste/cobalt Schiff base composite electrode. The electrooxidation of these compounds at bare electrode is sluggish, and there is no suitable peak separation between them. However, using cobalt methyl salophen as modifier, two well-defined anodic waves with a considerable enhancement in the peak current and a remarkable peak potential separation near 315 mV are obtained. It can improve the kinetics of electron transfer for both compounds remarkably. All these improvements are created because of the electrocatalytic property of cobalt Schiff base complex. The effect of some parameters such as pH and scan rates were studied. All the anodic peak currents for the oxidation of ascorbic acid and uric acid shifted toward more negative potential with an increase in pH, revealing that protons have taken part in their electrode reaction processes. The best peak separation with appropriate current was obtained for pH 4.0. A linear range of 5.0?×?10?4 to 1.0?×?10?8 and 1.0?×?10?3 to 1.0?×?10?8 M with detection limit of 8.0?×?10?9 and 8.0?×?10?9 M was obtained for ascorbic acid and uric acid using differential pulse voltammetry at the surface of modified electrode, respectively. Analytical utility of the modified electrode has been examined successfully using human urine samples and vitamin C commercial tablets.  相似文献   

9.
ABSTRACT

In the present study, a simple, cheap and sensitive electrochemical method based on a cathodically pretreated boron-doped diamond (CPT-BDD) electrode is described for the detection of triclosan with the cationic surfactant (cetyltrimethylammonium bromide, CTAB) media. The oxidation of triclosan was irreversible and exhibited an adsorption controlled process. The sensitivity of the adsorptive stripping voltammetric measurements was significantly improved with addition of CTAB. Using square-wave stripping mode, a linear response was obtained for triclosan determination in Britton-Robinson buffer solution at pH 9.0 containing 2.5 × 10?4 M CTAB at around + 0.67 V (vs. Ag/AgCl) (after 30 s accumulation at open-circuit condition). The method could be used in the range of 0.01–1.0 μg mL?1 (3.5 × 10?8–3.5 × 10?6 M), with a detection limit of 0.0023 μg mL?1 (7.9 × 10?9 M). The feasibility of the proposed method for the determination of triclosan in water samples was checked in spiked tap water.  相似文献   

10.
《Analytical letters》2012,45(16):2436-2444
The work demonstrates a simple method for sensitive detection of Ca2+ ion by electrochemical response of alizarin red S (ARS) and Ca-ARS at a gold nanoparticle modified glassy carbon electrode (GCE). In the 0.1 M KOH, a sensitive reduction peak was observed at ?0.795 V at the gold nanoparticles modified electrode. The peak currents were proportional to the concentrations of Ca2+ ion in the range of 2.0 × 10?7 M–1.2 × 10?4 M. For the different pulse voltammetry (DPV) methods, the detection limit was 2.57 × 10?8 M. The reaction mechanism was primarily determined by cyclic voltammetry, and the experimental results showed that the electrode processes were quasireversible responses of ARS and irreversible responses of ARS-Ca. In addition, the method was simple, fast, precise, and was used in the determination of calcium in blood serum with satisfactory results.  相似文献   

11.
《Analytical letters》2012,45(16):2665-2682
Abstract

The oxidation of theophylline was studied at a carbon paste electrode in the presence of cetyltrimethyl ammonium bromide by cyclic and differential pulse voltammetry. The results indicated that the electrochemical responses of theophylline are apparently improved by cetyltrimethyl ammonium bromide, due to the enhanced accumulation of theophylline at carbon paste electrode surface. Under optimal conditions the peak current was proportional to theophylline concentration in the range of 8.0 × 10?7 to 2.0 × 10?4 M with a detection limit of 1.85 × 10?7 M by differential pulse voltammetry. The proposed method was applied to the determination of theophylline in tablet and urine samples.  相似文献   

12.
Preconcentration is achieved by adsorption of a palladium-dimethylglyoxime complex on a hanging mercury drop electrode. Optimal conditions area stirred acetate buffer solution (pH 5.15) containing 2 × 10?4 M dimethylglyoxime and an accumulation potential of —0.20 V. The height of the stripping peak in a negative-going linear scan is linearly dependent on palladium concentration and preconcentration time (over the ranges 0–16 μg l?1 and 0–300 s, respectively). For a 10-min preconcentration time, the detection limit is 20 ng l?1 (2.1 × 10?10 M). Possible interferences by other trace metals are investigated. Palladium added to seawater samples was easily quantified.  相似文献   

13.
A sensitive electroanalytical method for the determination of anticancer drug etoposide (ETP) using adsorptive stripping differential pulse voltammetry (AdSDPV) at a multi-walled carbon nanotube-modified glassy carbon electrode (MWCNT-modified GCE) is presented. The surface morphology of modified electrode was characterized by scanning electron microscopy. The effects of accumulation time and potential, pH, scan rate, and amount of MWCNT suspension were investigated. The calibration curve was linear in the concentration range of 2.0?×?10?8–2.0?×?10?6 M with the detection limit of 5.4?×?10?9 M. The reproducibility of the peak current was found at 1.55 % (n?=?5) RSD value in pH 6.0 Britton–Robinson buffer for the MWCNT-modified GCE. The method was then successfully utilized for the determination of ETP in pharmaceutical dosage form, and a recovery of 99.55 % was obtained. The possible oxidation mechanism of ETP was also discussed. The proposed electroanalytical method using MWCNT-modified GCE is the most sensitive method for the determination of ETP with lowest limit of detection in the previously published electrochemical methods.  相似文献   

14.
《Analytical letters》2012,45(4):582-592
Abstract

A new type of gold nanoparticles–attached indium tin oxide electrode was made. By SEM and EDS, the as‐prepared gold nanoparticles–modified ITO electrode was characterized. This modified electrode has been used for the determination of pirarubicin (THP) in urine by cyclic voltammetry. Compared to a bare ITO electrode, the modified electrode exhibited a marked enhancement in the current response. Liner calibration curves are obtained in the range 5×10?9mol/L~1.5×10?6 mol/L with a detection limit of 1×10?9 mol/L. The percentage of the recoveries ranged from 99.3% to 106.3%. The practical analytic utility of the method is illustrated by quantitative determination of THP in urine.  相似文献   

15.
In this paper, a simple, convenient and sensitive electrochemical method has been developed for the determination of C.I. Direct Red 80. A gold nanoparticle modified carbon paste electrode was fabricated and used for study and sensitive determination of Direct Red 80 by cyclic voltammetry and differential pulse voltammetry. The overall analysis involved a two-step procedure: an accumulation step under open-circuit conditions, followed by voltammetric measurements of Direct Red 80 in a 0.1?M phosphate buffer solution at pH?=?3.0. The experimental conditions, such as the medium, pH and accumulation time, were optimised. The oxidation peak current was proportional to the concentration of Direct Red 80 from 5.0?×?10?8 to 5.0?×?10?7?M and 5.0?×?10?7 to 3.0?×?10?6?M, and the detection limit was 1.15?×?10?8?M (S/N?=?3). The proposed method was used to detect Direct Red 80 in natural water and sewage with good accuracy.  相似文献   

16.
The applicability of the carbon paste electrode to the determination of trace quantities of mercury has been investigated in a base electrolyte of 0.1 N KSCN + 0.025 N HCl containing 25 ng/ml copper. The detection limit of the mercury determination has a value near 2.5 ng/ml (1.25×10?8 M), if pre-electrolysis is carried out 10 min at ?1.0 V and the current voltage curve is registered with a scan rate of 16.7 mV/sec between ?0.5 and +0.5 V. The peak height is directly proportional to the concentration in the range from 1.25×10?8 to 1.25×10?6 M. With appropriate preconditioning the carbon paste electrode can be used for several measurements without renewing the surface.  相似文献   

17.
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   

18.
An electrochemical sensor has been constructed for the determination of adriamycin (ADM) that is based on a glassy carbon electrode modified with silver nanoparticles and multi-walled carbon nanotubes with carboxy groups. The modified electrode was characterized by scanning electron microscopy and exhibits a large enhancement of the differential pulse voltammetric response to ADM. Signals are linear with the concentrations of ADM in the range from 8.2?×?10?9 M to 19.0?×?10?9 M, with a detection limit of 1.7?×?10?9 M. The sensor is highly reproducible and exhibits excellent stability. It was to detect calf thymus DNA.  相似文献   

19.
Cathodic stripping voltammetry of selenium(IV) in 0.1 M hydrochloric acid media yielded a nonlinear calibration graph for the concentration range 10?9?10?8 M. In this concentration range, adsorptive stripping voltammetry based on adsorption of the selenium/3,3′-diaminobenzidine complex on the surface of the hanging mercury drop electrode at the deposition potential of +0.05 V (vs. SCE) is more convenient. A linear calibration graph is obtained for selenium concentrations of 3×10?9?3×10?8 M, with an accumulation time of 300 s.  相似文献   

20.
《Analytical letters》2012,45(12):1913-1931
Abstract

A voltammetric study of the oxidation of fexofenadine HCl (FEXO) has been carried out at the glassy carbon electrode. The electrochemical oxidation of FEXO was investigated by cyclic, linear sweep, differential pulse (DPV), and square wave (SWV) voltammetry using glassy carbon electrode. The oxidation of FEXO was irreversible and exhibited diffusion‐controlled process depending on pH. The dependence of intensities of currents and potentials on pH, concentration, scan rate, nature of the buffer was investigated. Different parameters were tested to optimize the conditions for the determination of FEXO. For analytical purposes, a very well resolved diffusion‐controlled voltammetric peak was obtained in Britton‐Robinson buffer at pH 7.0 with 20% constant amount of methanol for DPV and SWV techniques. The linear response was obtained in supporting electrolyte in the ranges of 1.0×10?6–2.0×10?4 M with a detection limit of 6.6×10?9 M and 5.76×10?8 M and in serum samples in the ranges of 2.0×10?6–1.0×10?4 M with a detection limit of 8.08×10?8 M and 4.97×10?8 M for differential pulse and square wave voltammetric techniques, respectively. Only square wave voltammetric technique can be applied to the urine samples, and the linearity was obtained in the ranges of 2.0×10?6–1.0×10?4 M with a detection limit of 2.00×10?7 M. Based on this study, simple, rapid, selective and sensitive two voltammetric methods were developed for the determination of FEXO in dosage forms and biological fluids. For the precision and accuracy of the developed methods, recovery studies were used. The standard addition method was used for the recovery studies. No electroactive interferences were found in biological fluids from the endogenous substances and additives present in tablets.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号