Electrodes with extremely high hydrogen overvoltages as substrate electrodes for stripping analysis based on bismuth-coated electrodes

Hydrogen evolution bothers stripping analysis significantly. Dioctyl phthalate-based carbon paste electrode exhibits extremely wide cathodic potential window. It is explored as a powerful substrate electrode to solve the problem of hydrogen evolution and further improve reproducibility for stripping analysis using bismuth-coated electrodes for the first time. It was successfully applied to the simultaneous determination of Zn²⁺, Cd²⁺, and Pb²⁺. Linear responses are obtained for Zn²⁺ in the range of 10–100 μg L⁻¹ and for Pb²⁺ and Cd²⁺ in the range of 5–100 μg L⁻¹. The detection limits for Zn²⁺, Cd²⁺, and Pb²⁺ are 0.1 μg L⁻¹, 0.22 μg L⁻¹ and 0.44 μg L⁻¹, respectively. The method has been successfully applied to the determination of Zn²⁺, Cd²⁺, and Pb²⁺ in waste water samples. The detection strategy based on the combination of dioctyl phthalate-based carbon paste electrode and bismuth-coated electrodes holds great promise for stripping analysis.     

Nafion/2,2'-bipyridyl-modified bismuth film electrode for anodic stripping voltammetry

This paper describes the fabrication, characterisation and the application of a Nafion/2,2′-bipyridyl/bismuth composite film-coated glassy carbon electrode (NC(Bpy)BiFE) for the anodic stripping voltammetric determination of trace metal ions (Zn²⁺, Cd²⁺ and Pb²⁺). The NC(Bpy)BiFE electrode is prepared by first applying a 2.5 mm³ drop of a coating solution containing 0.5 wt% Nafion and 0.1% (w/v) 2,2′-bipyridil (Bpy) onto the surface of a glassy carbon electrode, while the Bi film was plated in situ simultaneously with the target metal ions at −1.4 V. The main advantage of the polymer coated bismuth film electrode is that the sensitivity of the stripping responses is increased considerably due to the incorporation of the neutral chelating agent of 2,2′-bipyridyl (Bpy) in the Nafion film, while the Nafion coating improved the mechanical stability of the bismuth film and its resistance to the interference of surfactants. The key experimental parameters relevant to both the electrode fabrication and the voltammetric measurement were optimized on the basis of the stripping signals. With a 2 min deposition time in the presence of oxygen, linear calibration curves were obtained in a wide concentration range (about 2-0.001 μM) with detection limits of 8.6 nM (0.56 μg dm⁻³) for Zn²⁺, 1.1 nM (0.12 μg dm⁻³) for Cd²⁺ and 0.37 nM (0.077 μg dm⁻³) for Pb²⁺. For nine successive preconcentration/determination/electrode renewal experiments the standard deviations were between 3 and 5% at 1.2 μM for zinc and 0.3-0.3 μM concentration level for lead and cadmium, respectively, and the method exhibited excellent selectivity in the presence of the excess of several potential interfering metal ions. The analytical utility of the stripping voltammetric method elaborated was tested in the assay of heavy metals in some real samples and the method was validated by ICP-MS technique.     

Ultrasensitive and simultaneous detection of heavy metal ions based on three-dimensional graphene-carbon nanotubes hybrid electrode materials

A green and facile method was developed to prepare a novel hybrid nanocomposite that consisted of one-dimensional multi-walled carbon nanotubes (MWCNTs) and two-dimensional graphene oxide (GO) sheets. The as-prepared three-dimensional GO–MWCNTs hybrid nanocomposites exhibit excellent water-solubility owing to the high hydrophilicity of GO components; meanwhile, a certain amount of MWCNTs loaded on the surface of GO sheets through π–π interaction seem to be “dissolved” in water. Moreover, the graphene(G)-MWCNTs nanocomposites with excellent conductivity were obtained conveniently by the direct electrochemical reduction of GO–MWCNTs nanocomposites. Seeing that there is a good synergistic effect between MWCNTs and graphene components in enhancing preconcentration efficiency of metal ions and accelerating electron transfer rate at G-MWCNTs/electrolyte interface, the G-MWCNTs nanocomposites possess fast, simultaneous and sensitive detection performance for trace amounts of heavy metal ions. The electrochemical results demonstrate that the G-MWCNTs nanocomposites can act as a kind of practical sensing material to simultaneously determine Pb²⁺ and Cd²⁺ ions in terms of anodic stripping voltammetry (ASV). The linear calibration plots for Pb²⁺ and Cd²⁺ ranged from 0.5 μg L⁻¹ to 30 μg L⁻¹. The detection limits were determined to be 0.2 μg L⁻¹ (S/N = 3) for Pb²⁺ and 0.1 μg L⁻¹ (S/N = 3) for Cd²⁺ in the case of a deposition time of 180 s. It is worth mentioning that the G-MWCNTs modified electrodes were successfully applied to the simultaneous detection of Cd²⁺ and Pb²⁺ ions in real electroplating effluent samples containing lots of surface active impurities, showing a good application prospect in the determination of trace amounts of heavy metals.     

Comparative study of graphene nanosheet- and multiwall carbon nanotube-based electrochemical sensor for the sensitive detection of cadmium

A novel nanocomposite was obtained through the controlled surface modification of graphene nanosheets (nanographene) with Nafion by ultrasonic oscillation. The composite was used as an ultrasensitive platform for the detection of cadmium ions (Cd²⁺) by differential pulse anodic stripping voltammetry (DPASV) analysis. The performance of the nanographene-based sensor was systematically compared with that of a multiwall carbon nanotube (MWCNT)-modified sensor. The results indicate that the nanographene-based sensor exhibits significant advantages over the MWCNT-based sensor in terms of repeatability, sensitivity and limit of detection (LOD). The nanographene-based sensor displayed superior analytical performance over a linear range of Cd²⁺ concentrations from 0.25 μg L⁻¹ to 5 μg L⁻¹, with a LOD of 3.5 ng L⁻¹. This sensor was also used to systematically screen for 6 types of chemicals, including sodium salts, magnesium salts and zinc salts. It was observed that the sensor could successfully differentiate cadmium ions from interferents (magnesium salts, zinc salts, etc.). The nanographene-based sensor was also demonstrated to be a promising and reliable tool for the rapid detection of cadmium existing in tap water and for the rapid on-site analysis of critical pollution levels of cadmium.     

Voltammetric determination of Cd2+ based on the bifunctionality of single-walled carbon nanotubes-Nafion film

In the presence of Nafion, single-walled carbon nanotubes (SWNTs) were easily dispersed into ethanol, resulting in a homogeneous SWNTs/Nafion suspension. After evaporating ethanol, a SWNTs/Nafion film with bifunctionality was constructed onto glassy carbon electrode (GCE) surface. Attributing to the strong cation-exchange ability of Nafion and excellent properties of SWNTs, the SWNTs/Nafion film-coated GCE remarkably enhances the sensitivity of determination of Cd²⁺. Based on this, an electrochemical method was developed for the determination of trace levels of Cd²⁺ by anodic stripping voltammetry (ASV). In pH 5.0 NaAc-HAc buffer, Cd²⁺ was firstly exchanged and adsorbed onto SWNTs/Nafion film surface, and then reduce at −1.10 V. During the positive potential sweep, reduced cadmium was oxidized, and a well-defined stripping peak appeared at −0.84 V, which can be used as analytical signal for Cd²⁺. The linear range is found to be from 4.0 × 10⁻⁸ to 4.0 × 10⁻⁶ mol L⁻¹, and the lowest detectable concentration is estimated to be 4.0 × 10⁻⁹ mol L⁻¹. Finally, this method was successfully employed to detect Cd²⁺ in water samples.     

Synthesis of a novel electrode material containing phytic acid-polyaniline nanofibers for simultaneous determination of cadmium and lead ions

The development of nanostructured conducting polymers based materials for electrochemical applications has attracted intense attention due to their environmental stability, unique reversible redox properties, abundant electron active sites, rapid electron transfer and tunable conductivity. Here, a phytic acid doped polyaniline nanofibers based nanocomposite was synthesized using a simple and green method, the properties of the resulting nanomaterial was characterized by electrochemical impedance spectroscopy (EIS), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS). A glassy carbon electrode modified by the nanocomposite was evaluated as a new platform for the simultaneous detection of trace amounts of Cd²⁺ and Pb²⁺ using differential pulse anodic stripping voltammetry (DPASV). The synergistic contribution from PANI nanofibers and phytic acid enhances the accumulation efficiency and the charge transfer rate of metal ions during the DPASV analysis. Under the optimal conditions, good linear relationships were obtained for Cd²⁺ in a range of 0.05–60 μg L⁻¹, with the detection limit (S/N = 3) of 0.02 μg L⁻¹, and for Pb²⁺ in a range of 0.1–60 μg L⁻¹, with the detection limit (S/N = 3) of 0.05 μg L⁻¹. The new electrode was successfully applied to real water samples for simultaneous detection of Cd²⁺ and Pb²⁺ with good recovery rates. Therefore, the new electrode material may be a capable candidate for the detection of trace levels of heavy metal ions.     

Determination of dissolved sulphides in waste water samples by flow-through stripping chronopotentiometry with a macroporous mercury-film electrode

Sulphides in water samples were determined by stripping chronopotentiometry in a computer controlled flow system with a flow-through electrochemical cell. The working electrode was a porous glassy carbon electrode coated with Nafion and mercury. The sample was diluted with 0.1 mol L⁻¹ NaOH and analysed. Sulphides in the sample were collected in the porous electrode as mercury sulphide and then stripped by a current of −500 μA. The limit of detection was found to be 1.6 μg L⁻¹ and 0.5 μg L⁻¹ for 1 mL and 5 mL of preconcentrated sample, respectively. The linear range for 1 mL sample was found to be 5-400 μg L⁻¹. The repeatability and reproducibility was found to be 2.6% and 4.8%, respectively. The method was applied to analyses of waste water samples from a tannery.     

Determination of Trace Lead and Cadmium in Water Samples by Anodic Stripping Voltammetry with a Nafion‐Ionic Liquid‐Coated Bismuth Film Electrode

A new chemically modified bismuth film electrode coated with an ionic liquid [(1‐ethyl‐3‐methylimidazolium tetracyanoborate (EMIM TCB)] and Nafion was developed for the simultaneous determination Pb²⁺ and Cd²⁺ by anodic stripping voltammetry. Compared with conventional bismuth film electrodes, this electrode exhibited greatly improved electrochemical activity for Pb²⁺ and Cd²⁺ detection due to the unique properties of Nafion polymer and ionic liquid. The key experimental parameters related to the fabrication of the electrode and the voltammetric measurements were optimized on the basis of the stripping signals, where the peak currents increased linearly with the metal concentrations in a range of 10–120 µg L^?1 with a detect limit of 0.2 µg L^?1 for Pb²⁺, and 0.5 µg L^?1 for Cd²⁺ for 120s deposition. High reproducibility was indicated from the relative standard deviations (1.9 and 2.5 %) for nine repetitive measurements of 20 µg L^?1 Pb²⁺ and Cd²⁺, respectively. In addition, the surface characteristics of the modified BiFE were investigated by scanning electron microscopy (SEM), and results showed that fibril‐like bismuth nanostructures were formed on the porous Nafion polymer matrix. Finally, the developed electrode was applied to determine Pb²⁺ and Cd²⁺ in water samples, indicating that this electrode was sensitive, reliable and effective for the simultaneous determination of Pb²⁺ and Cd²⁺.     

Photoelectrochemical determination of inorganic mercury in aqueous solutions

An analytical method using an optical probe in a photoelectrochemical cell for the sensitive and selective determination of aqueous Hg²⁺ is presented. A previously synthesized Hg²⁺ selective chemosensor, proven to be Hg²⁺ sensitive up to 2 μg L⁻¹, has been immobilized onto indium tin oxide (ITO) electrodes in a composite form with polyaniline. The coated ITO electrode was placed in a photoelectrochemical cell under closed circuit conditions in which the optical recognition of the chemosensor was converted to a measurable signal. A composite of the fluorescent chemosensor, Rhodamine 6G derivative (RS), and polyaniline (PANI) was immobilized on ITO glass plates and subjected to photovoltage measurements in the absence and presence of Hg²⁺. The optical responses of the coated electrode were used to determine the sensitivity and selectivity of the immobilized sensor to Hg²⁺ in the presence of background ions. The optical response of the PANI-dye coated electrode increased linearly with increasing Hg²⁺ concentration in the range 10-150 μg L⁻¹, with a detection limit of 6 μg L⁻¹.     

Mercury-free simultaneous determination of cadmium and lead at a glassy carbon electrode modified with multi-wall carbon nanotubes

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.     

Simultaneous determination of Mn(II), Cu(II) and Fe(III) as 2-(5′-bromo-2′-pyridylazo)-5-diethylaminophenol complexes by adsorptive cathodic stripping voltammetry at a carbon paste electrode

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.     

Determination of cadmium with a sequential injection lab-on-valve by anodic stripping voltammetry using a nafion coated bismuth film electrode

This work exploited a sequential injection lab-on-valve (LOV) system for the determination of cadmium by anodic stripping voltammetry (ASV). A miniaturized electrochemical flow cell (EFC) was fabricated in LOV, in which a nafion coated bismuth film electrode was used as working electrode. The cadmium was electrodeposited on the electrode surface in bismuth solution, and measured with the subsequential stripping scan. Under optimal conditions, the proposed system responded linearly to cadmium concentrations in a range 2.0-100.0 μg L⁻¹. The detection limit of this method was found to be 0.88 μg L⁻¹. By loading a sample volume of 800 μL, a sampling frequency of 22 determinations h⁻¹ was achieved. The repeatability expressed as relative standard derivation (R.S.D.) was 3.65% for 20 μg L⁻¹ cadmium (n = 11). The established method was applied to analysis of trace cadmium in environmental water samples and the spiked recoveries were satisfactory.     

Bifunctional polydopamine@Fe3O4 core–shell nanoparticles for electrochemical determination of lead(II) and cadmium(II)

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.     

Square wave voltammetric determination of nitrofurantoin in pharmaceutical formulations on highly boron-doped diamond electrodes at different boron-doping contents

The influence of the boron-doping levels in boron-doped diamond film electrodes on the electrochemical response of nitrofurantoin (NFT) and the development of an electroanalytical procedure for NFT determination were investigated. The investigations were carried out using the techniques of cyclic voltammetry and square wave voltammetry on diamond film electrodes with different boron-doping levels (i.e., 5000, 10,000 and 20,000 mg L⁻¹). The level of boron-doping in the diamond film electrodes influenced the electrochemical reduction of NFT. The appropriate cyclic voltammetric response of NFT was obtained with Britton-Robinson buffer at pH 4 and for diamond films doped with 10,000 and 20,000 mg L⁻¹ of boron. These two films were selected for the development of the electroanalytical procedure. The use of square wave voltammetry with the optimized parameters demonstrated a good linear relationship between the peak current and the NFT concentration for a wide range of concentration. The lower limit of detection for the electrodes doped with 10,000 and 20,000 mg L⁻¹ of boron were 2.69 × 10⁻⁸ mol L⁻¹ (6.40 μg L⁻¹) and 8.15 × 10⁻⁹ mol L⁻¹ (1.94 μg L⁻¹), respectively, while the lower limits of quantification were 8.96 × 10⁻⁸ mol L⁻¹ (21.33 μg L⁻¹) and 2.72 × 10⁻⁸ mol L⁻¹ (6.47 μg L⁻¹), respectively. The applicability of the proposed procedure was tested using a commercial pharmaceutical formulation of NFT, and the results were compared with the procedure recommended by the British Pharmacopeia. The proposed procedure was sensitive, accurate and precise for analysis of NFT and did not require complex preparations or renovations of the electrode surface. This presents the advantage of eliminating mercury waste and minimizing the adsorptive problems related to the use of other electrodic solid surfaces.     

Sequential injection monosegmented flow voltammetric determination of cadmium and lead using a bismuth film working electrode

A cost-effective sequential injection monosegmented flow analysis (SI-MSFA) with anodic stripping voltammetric (ASV) detection has been developed for determination of Cd(II) and Pb(II). The bismuth film working electrode (BiFE) was employed for accumulative preconcentration of the metals by applying a fixed potential of −1.10 V versus Ag/AgCl electrode for 90 s. The SI-MSFA provides a convenient means for preparation of a homogeneous solution zone containing sample in an acetate buffer electrolyte solution and Bi(III) solution for in situ plating of BiFE, ready for ASV measurement at a flow through thin layer electrochemical cell. Under the optimum conditions, linear calibration graphs in range of 10-100 μg L⁻¹ of both Cd(II) and Pb(II) were obtained with detection limits of 1.4 and 6.9 μg L⁻¹ of Cd(II) and Pb(II), respectively. Relative standard deviations were 2.7 and 3.1%, for 11 replicate analyses of 25 μg L⁻¹ Cd(II) and 25 μg L⁻¹ Pb(II), respectively. A sample throughput of 12 h⁻¹ was achieved with low consumption of reagent and sample solutions. The system was successfully applied for analysis of water samples collected from a draining pond of zinc mining, validating by inductively coupled plasma-optical emission spectroscopy (ICP-OES) method.     

Simultaneous determination of cadmium (II) and lead (II) with clay nanoparticles and anthraquinone complexly modified glassy carbon electrode

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.     

Preparation of a carbon ceramic electrode modified by 4-(2-pyridylazo)-resorcinol for determination of trace amounts of silver

A 4-(2-pyridylazo)-resorcinol (PAR)-modified carbon ceramic electrode (CCE) prepared by the sol-gel technique has been reported for the first time in this paper. By immersing the CCE in aqueous solution of PAR (0.001 mol L⁻¹), after a short period of time, a thin film of PAR was rapidly formed on the surface of the electrode due to its strong adsorption properties. A differential pulse anodic stripping voltammetric (DPASV) method was developed for determination of Ag(I) at the modified carbon ceramic electrode. The analysis procedure consisted of an open circuit accumulation step in a sample solution which was continuously stirred for 12 min. This was followed by replacing the medium with a clean solution where the accumulated Ag(I) was reduced for 15 s in −0.6 V. Then, the potential was scanned from −0.2 to +0.2 V to obtain the voltammetric peak. The detection limit of silver(I) was 0.123 μg L⁻¹, and for seven successive determinations of 10, 100 and 200 μg L⁻¹ Ag(I), the relative standard deviations were 2.1, 1.4 and 1.03%, respectively. The calibration curve was linear for 0.5-300 μg L⁻¹ silver(I). The procedure was applied to determine silver(I) in X-ray photographic films and super-alloy samples.     

Bismuth-dispersed xerogel-based composite films for trace Pb(II) and Cd(II) voltammetric determination

We report for the first time the synthesis of bismuth-modified (3-mercaptopropyl) trimethoxysilane (MPTMS) and its application for the determination of lead and cadmium by anodic stripping voltammetry. Xerogels made from bismuth-modified MPTMS and mixtures of it with tetraethoxysilane, under basic conditions (NH₃·H₂O), were characterized with scanning electron microscopy, energy dispersive spectroscopy, infrared spectroscopy and electrochemical methods. Bismuth-modified xerogels were mixed with 1.5% (v/v) Nafion in ethanol and applied on glassy carbon electrodes. During the electrolytic reductive deposition step, the bismuth compound on the electrode surface was reduced to metallic bismuth. The target metal cations were simultaneously reduced to the respective metals and were preconcentrated on the electrode surface by forming an alloy with bismuth. Then, an anodic voltammetric scan was applied in which the metals were oxidized and stripped back into the solution; the voltammogram was recorded and the stripping peak heights were related to the concentration of Cd(II) and Pb(II) ions in the sample. Various key parameters were investigated in detail and optimized. The effect of potential interferences was also examined. Under optimum conditions and for preconcentration period of 4 min, the 3σ limit of detection was 1.3 μg L⁻¹ for Pb(II) and 0.37 μg L⁻¹ for Cd(II), while the reproducibility of the method was 4.2% for lead (n = 5, 10.36 μg L⁻¹ Pb(II)) and 3.9% for cadmium (n = 5, 5.62 μg L⁻¹ Cd(II)). Finally, the sensors were applied to the determination of Cd(II) and Pb(II) ions in water samples.     

Ultra trace adsorptive stripping voltammetric determination of atrazine in soil and water using mercury film electrode

In situ mercury film electrode produced in the presence of thiocyanate has been shown extremely useful for highly sensitive adsorptive stripping voltammetric measurements of atrazine down to sub-μg L⁻¹ level. Operational parameters have been optimized and the stripping voltammetric performance has been investigated using square wave scans. The adsorptive stripping response is linear over the range of 0.5-60 μg L⁻¹ atrazine, with a detection limit of 0.024 μg L⁻¹. The method has been applied to the determination of atrazine in soil and water samples.