Selective solid phase extraction of palladium by adsorption of its 5(p-dimethylaminobenzylidene)rhodanine complex on silica-PEG as a new adsorbent

The nickel(II) complex of a deoxyribonucleic acid (DNA-Ni²⁺) was directly electrodeposited on the surface of a glassy carbon electrode (GCE) to give a DNA-Ni/GCE electrode. It was investigated in terms of its capability of electro-oxidizing methanol in alkaline medium. It exhibits stable redox behavior of the Ni²⁺/Ni³⁺ couple by cyclic voltammetry. The DNA-Ni²⁺ membrane showed excellent electrocatalytic suitability for the electro-oxidation of methanol, is stable and responds reproducibly. The linear range for the detection of methanol in alkaline medium is from 8.0 µM to 2.4 mM, and the limit of detection is 2.0 µM (at a signal-to-noise ratio of 3).     

Addition of porous cuprous oxide to a Nafion film strongly improves the performance of a nonenzymatic glucose sensor

The direct electrocatalytic oxidation of glucose in alkaline medium at an electrode modified with microcubes of porous cuprous oxide is reported. Compared to the glassy carbon electrode, a substantial increase in the efficiency of the electrocatalytic oxidation of glucose is observed starting at around +0.20 V (vs. Ag/AgCl). The pH dependence of the response was examined by cyclic voltammetry. This non-enzymatic amperometric sensor may be used for non-enzymatic detection of glucose with a high and reproducible sensitivity of 10.95 μA per mM at a potential of +0.40 V, with response times of <3 s, a linear range from 2.0 to 350 μM, and a detection limit of 1.3 μM. The porous microcubes are conveniently prepared, and display high sensitivity and repeatability.     

A sensitive amperometric hydrogen peroxide sensor based on thionin/EDTA/carbon nanotubes—chitosan composite film modified electrode

A sensitive amperometric sensor has been constructed for the determination of hydrogen peroxide (HP). It is based on a glassy carbon electrode modified with a composite made from thionin, EDTA, multiwalled carbon nanotubes, and chitosan. Thionin was covalently immobilized on the surface of the electrode. The sensor exhibits a powerful electrocatalytic activity for the reduction of HP. The amperometric signal is proportional to the concentration of HP in the range from 0.2 μM to 85.0 μM, with a detection limit of 0.065 μM. The sensor displays excellent selectivity, good reproducibility and long-term stability.     

Nickel electrode modified by N,N-<Emphasis Type="Italic">bis</Emphasis>(salicylidene)phenylenediamine (Salophen) as a catalyst for methanol oxidation in alkaline medium

The electrocatalytic oxidation of methanol studied at the surface of nickel disc electrode coated with N,N-bis(salicylidene)phenylenediamine (Salophen) legend in 0.10 M NaOH solution using cyclic voltammetry. The results showed that the Ni-salophen layer formed at the surface of electrode behaves as an efficient electrocatalyst for the oxidation of methanol in alkaline medium. The thermal analysis of Ni-salophen complex studied at temperature ranges 0–800°C in argon atmosphere. Also, FTIR was employed to prove the formation of complex on the modified electrode surface. Moreover, the effects of various parameters such as oven temperature, methanol concentration, NaOH concentration and media temperature on electro-oxidation of methanol were investigated. The kinetic parameters such as activation energy and Tafel slope were calculated for methanol oxidation on the modified electrode surface. Published in Elektrokhimiya in Russian, 2009,, 2009, Vol. 45, No. 2, pp. 203–210. The text was submitted by author in English.     

A highly sensitive nonenzymatic glucose sensor based on nickel oxide–carbon nanotube hybrid nanobelts

In this study, we demonstrated a highly sensitive electrochemical sensor for the determination of glucose in alkaline aqueous solution by using nickel oxide single-walled carbon nanotube hybrid nanobelts (NiO–SWCNTs) modified glassy carbon electrode (GCE). The hybrid nanobelts were prepared by the deposition of SWCNTs onto the Ni(SO₄)_0.3(OH)_1.4 nanobelt surface, followed by heat treatment at different temperatures ranging from 400 °C to 600 °C. The NiO–SWCNTs hybrid nanobelts modified electrode prepared at 500 °C displays enhanced electrocatalytic activity towards glucose oxidation, revealing a synergistic effect between the NiO and the deposited SWCNTs. The as-fabricated nonenzymatic glucose sensor exhibits excellent glucose sensitivity (2,980 μA cm^?2 mM^?1), lower detection limit (0.056 μM, signal/noise [S/N] ratio?=?3), and wider linear range (0.5–1,300 μM). Moreover, the sensor has been successfully used for the assay of glucose in serum samples with good recovery, ranging from 96.4 % to 102.4 %.     

Electrocatalytic oxidation of methanol by ZSM-5 nanozeolite-modified carbon paste electrode in alkaline medium

Development of a novel modified electrode for electrocatalytic oxidation of methanol in order to decrease overvoltage is importance. In this paper, carbon paste electrode (CPE) was modified by ZSM-5 nanozeolite. The average diameter of used nanozeolite was 97 nm. Ni²⁺ ions were incorporated to the nanozeolite by immersion of the modified electrode in a 0.1 M nickel chloride solution. Then, electrochemical studies of this electrode were performed by using cyclic voltammetry(CV) in alkaline medium. This modified electrode was used as an anode for the electrocatalytic oxidation of methanol in 0.1 M of NaOH solution. The obtained data demonstrated that ZSM-5 nanozeolite at the surface of CPE improves catalytic efficiency of the dispersed nickel ions toward methanol oxidation. The values of electron transfer coefficient, charge-transfer rate constant, and the electrode surface coverage are obtained 0.61, 0.2342 s^?1, and 4.33 × 10^?8 mol cm^?2, respectively. Also, the mean value of catalytic rate constant between the methanol and redox sites of electrode and diffusion coefficient were found to be 2.54 × 10⁴ cm³ mol^?1 s^?1 and 1.85 × 10^?8 cm² s^?1, respectively. Obtained results from both CV and chronoamperometric techniques indicated that the electrode reaction is a diffusion-controlled process.     

A sensitive and selective nitrite sensor based on a glassy carbon electrode modified with gold nanoparticles and sulfonated graphene

We describe a highly sensitive and selective amperometric sensor for the determination of nitrite. A glassy carbon electrode was modified with a composite made from gold nanoparticles (AuNPs) and sulfonated graphene (SG). The modified electrode displays excellent electrocatalytic activity in terms of nitrite oxidation by giving much higher peak currents (at even lower oxidation overpotential) than those found for the bare electrode, the AuNPs-modified electrode, and the SG-modified electrode. The sensor has a linear response in the 10 μM to 3.96 mM concentration range, a very good detection sensitivity (45.44 μA mM^?1), and a lower detection limit of 0.2 μM of nitrite. Most common ions and many environmental organic pollutants do not interfere. The sensor was successfully applied to the determination of nitrite in water samples, and the results were found to be consistent with the values obtained by spectrophotometry.

Nickel–poly(o-aminophenol)-modified carbon paste electrode; an electrocatalyst for methanol oxidation

In this work, a modified carbon paste electrode consisting of Nickel dispersed in poly(ortho-aminophenol) was used for electrocatalytic oxidation of methanol in alkaline solution. A carbon paste electrode bulk modified with o-aminophenol was used for polymer preparation by cyclic voltammetry method; then, Ni(II) ions were incorporated by immersion of the modified electrode in 1 M Ni(II) ion solution at open circuit. The electrochemical characterization of this modified electrode exhibits stable redox behavior of the Ni(III)–Ni(II) couple. Electrocatalytic oxidation of methanol on the surface of modified electrode was investigated with cyclic voltammetry and chronoamperometry methods, and the dependence of the oxidation current and shape of cyclic voltammograms on methanol concentration and scan rate were discussed. Also, long-term stability of modified electrode for electrocatalytic oxidation of methanol was investigated.     

Nickel modified ionic liquid/carbon paste electrode for highly efficient electrocatalytic oxidation of methanol in alkaline medium

In this study, the electrocatalytic oxidation of methanol at nickel modified ionic liquid/carbon paste electrode (Ni/IL/CPE) in alkaline medium is presented. The ionic liquid, 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, is incorporated into the electrode as a binder. Electrochemical impedance spectroscopy is employed to evaluate the electron transfer rate of this electrode. Ni(II) ions are incorporated into the electrode by immersion of this electrode in 1.0?M nickel sulfate solution. Cyclic voltammetry and chronoamperometry techniques are used for the electrochemical study of this modified electrode in the absence and the presence of methanol. The effect of methanol concentration on the anodic peak current shows an increase in the anodic peak current up to 1.25?M. Current density of Ni/IL/CPE for methanol oxidation in alkaline media is investigated by comparison with some of the previously reported electrodes. Results show that this electrode exhibits a high efficient electrocatalytic activity toward the oxidation of methanol with the current density of 17.6?mA?cm^?2. The rate constant for chemical reaction between methanol and redox sites of electrode is calculated. This new proposed electrode is simple and efficient enough, and it can be widely used as anode in direct methanol fuel cell.     

Electro-oxidation of methanol catalysed by porous nanostructured Fe/Pd-Fe electrode in alkaline medium

Nanostructured Fe/Pd-Fe catalysts are prepared first by the deposition of Fe-Zn onto the Fe electrode surface, followed by replacement of the Zn by Pd at open circuit potential in a Pd-containing alkaline solution. The surface morphology and composition of coatings are determined by scanning electron microscopy and energy dispersive X-ray techniques. The results show that the Fe/Pd-Fe coatings are porous structure and the average particle size of Pd-Fe is low, in the range of 30–80 nm. The electrocatalytic activity and stability of Fe/Pd-Fe electrodes for oxidation of methanol are examined by cyclic voltammetry and chronoamperometry techniques. The new Fe/Pd-Fe catalyst has higher electrocatalytic activity and better stability for the electro-oxidation of methanol in an alkaline media than flat Pd and smooth Fe catalysts. The onset potential and peak potential on Fe/Pd-Fe catalysts are more negative than that on flat Pd and smooth Fe electrodes for methanol electro-oxidation. All results show that the nanostructured Fe/Pd-Fe electrode is a promising catalyst towards methanol oxidation in alkaline media for fuel cell applications.     

Electrocatalytic study of an electrode modified with Reactive Blue 4 dye covalently immobilized on amine-functionalized silica

In the present work, we investigated the immobilization and electrochemical behavior of Reactive Blue 4 dye on 3-aminopropyl-functionalized silica. The electrochemical behavior of the modified electrode and the electro-oxidation of dipyrone were studied by cyclic voltammetry. The modified electrode showed a well-defined redox coupling with a formal potential of 0.45 V (vs. saturated calomel reference electrode) assigned to anthraquinone/anthrahydroquinone redox process (pH?=?2). The modified electrode also demonstrated electrocatalytic activity and an increased peak current towards the oxidation of dipyrone at a reduced overall potential. The electrocatalytic process was found to be highly dependent on the pH of the supporting electrolyte. The voltammetric responses for dipyrone were linear in the concentration range of 49.9 to 440 μmol L^?1 at a pH of 2.0 with a detection limit and sensitivity of 22.0 μmol L^?1 and 0.0278 μA mmol L^?1, respectively.     

Amperometric sensor for ascorbic acid based on a glassy carbon electrode modified with gold-silver bimetallic nanotubes in a chitosan matrix

We report on an amperometric sensor for ascorbic acid (AA) that is based on highly dense gold-silver nanotubes in a chitosan film on a glassy carbon electrode. The nanotubes were synthesized by a poly(vinyl pyrrolidone)-mediated polyol method employing a replacement reaction with silver nanowires as templates, and were characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray diffraction. Under the optimal conditions, the sensor exhibits good electrocatalytic activity towards the oxidation of AA, and this enables the determination of AA in the 5 μM to 2 mM concentration range, with a detection limit at 2 μM (at an S/N of 3). The response time is 2 s. The sensor displays good reproducibility, selectivity, sensitivity, and long-term stability.

Synthesis of a Palladium-Graphene Material and Its Application for Formaldehyde Determination

A novel electrochemical sensor for formaldehyde determination was fabricated by using the Pd-graphene nanohybrides. Pd-graphene nanohybrids were prepared via a concise chemical reduction method. Raman spectroscopy, X-ray diffraction (XRD), and transmission electron microscopy (TEM) were used for the characterization of structure and morphology of the nanohybrids. The result showed that Pd nanoparticles were uniformly dispersed and were well-separated on the graphene sheets. The Pd-graphene nanohybrids were dissolved in Nafion and modified on the glassy carbon electrode to fabricate the electrochemical sensor. This proposed electrochemical sensor performed excellent electrocatalytic activity toward formaldehyde oxidation in alkaline medium. The peak current was linearly related to the formaldehyde concentration in the range of 7.75 µM to 62.0 µM with the detection limit of 3.15 µM. The highly sensitive and robust graphene based Pd nanohybrids sensor offers a promising and practical tool for formaldehyde sensing and chemical analysis.     

Electrocatalytic oxidation of methanol on a glassy carbon modified electrode by bis(1,2-phenylenediamine) nickel(II) complex

Electrocatalytic oxidation of methanol on a glassy carbon electrode coated with Ni(II)-(1,2-phenylendiamine)₂ (GC/NiOPD), conditioned by the potential recycling in a potential range of 100–650 mV (vs. SCE) is studied by cyclic voltammetry in an alkaline medium (0.10 M NaOH). The results show that the NiOPD layer formed at the surface of the electrode behaves as an efficient electrocatalyst for the oxidation of methanol in the alkaline medium via the Ni(III) species with a cross exchange reaction occurring throughout the layer at a low concentration of methanol. The effects of various parameters such as potential scan rates, methanol concentration and NiOPD surface concentration on the electro-oxidation of methanol are also investigated.     

Amperometric nonenzymatic glucose sensor based on a glassy carbon electrode modified with a nanocomposite made from nickel(II) hydroxide nanoplates and carbon nanofibers

We report on a highly sensitive and selective nonenzymatic glucose sensor based on a glassy carbon electrode modified with a composite prepared from nickel(II) hydroxide nanoplates and carbon nanofibers. The nanocomposite was characterized by scanning electron microscopy and powder X-ray diffraction. Electrodes modified with pure Ni(OH)₂ and with the nanocomposite were characterized by electrochemical impedance spectroscopy. Cyclic voltammetric and amperometric methods were used to investigate the catalytic properties of the modified electrodes for glucose electrooxidation in strongly alkaline solution. The sensor exhibits a wide linear range (from 0.001 to 1.2 mM), a low detection limit (0.76 μM), fast response time (< 5 s), high sensitivity (1038.6 μA?·?mM^?1?·?cm^?2), good reproducibility, and long operational stability. Application of the nonenzymatic sensor for monitoring glucose in real samples was also demonstrated.

Synthesis and characterisation of Ag-nanoparticles immobilised on ordered mesoporous carbon as an efficient sensing platform: application to electrocatalytic determination of hydrazine

In this study, a new strategy for the preparation of a modified glassy carbon electrode (GCE) based on a novel nano-sensing layer for the electrocatalytic oxidation of hydrazine was suggested. The suggested nano-sensing layer was prepared with the immobilisation of silver nanoparticles (AgNPs) on ordered mesoporous carbon. The morphology and properties of the prepared nanocomposite on the surface of GCE were characterised by scanning electron microscopy, transmission electron microscopy, N₂ adsorption-desorption, X-ray powder diffraction and electrochemical impedance spectroscopy. The electrochemical response characteristics of the modified electrode towards the target analyte were investigated by cyclic voltammetry. Under optimal experimental conditions, the suggested modified GCE showed excellent catalytic activity towards the electro-oxidation of hydrazine (pH = 7.5) with a significant increase in anodic peak currents in comparison with the unmodified GCE. By differential pulse voltammetry and amperometric methods, the suggested sensor demonstrated wide dynamic concentration ranges of 0.08–33.8 µM and 0.01–128 µM with the detection limit (S/N = 3) of 0.027 and 0.003 µM for hydrazine, respectively. The suggested hydrazine sensor was successfully applied for the highly sensitive determination of hydrazine in different real samples with satisfactory results.     

Carbohydrates electrocatalytic oxidation using CNT-NiCo-oxide modified electrodes

A new sensor for an amplified electrochemical detection of carbohydrates is proposed, where carbohydrates are oxidized by CNT-NiCo-oxide composite in basic solutions. Cyclic voltammograms of the modified electrode show a stable and well defined redox couple in alkaline media due to the synergy of Ni(II)/Ni(III) system with Co(II)/Co(III). The modified electrode shows excellent electrocatalytic activity towards monosaccharides oxidation at reduced overpotential in alkaline solutions. Six monosaccharides were determined amperometrically at the surface of this modified electrode with high sensitivity over a wide range of concentrations, from 0.02 up to 12.12 mM. Low detection limit of 5 μM for glucose could be obtained.     

Electrochemical behavior and voltammetric determination of L-tryptophan and L-tyrosine using a glassy carbon electrode modified with single-walled carbon nanohorns

We report a simple method for the direct and quantitative determination of L-tryptophan (Trp) and L-tyrosine (Tyr) using a glassy carbon electrode (GCE) modified with single-walled carbon nanohorns (SWCNHs). The SWCNH modified GCE exhibits high electrocatalytic activity towards the oxidation of both Trp and Tyr. It shows a linear response to Trp between 0.5 and 50 μM and to Tyr between 2 and 30 μM. The detection limits for Trp and Tyr are 50 nM and 400 nM, respectively. In addition, the modified GCE displays good selectivity and good sensitivity, thus making it suitable for the determination of Trp and Tyr in spiked serum samples.

Simultaneous Sensitive Determination of Dopamine and Uric Acid in the Presence of Excess Ascorbic Acid with a Magnetic Chitosan Microsphere/Thionine Modified Electrode

Magnetic chitosan microspheres (MCMS) and thionine were incorporated in a modified electrode for the simultaneous sensitive determination of dopamine (DA) and uric acid (UA). Due to the unique properties of the MCMS and the electron mediation of thionine, this modified electrode showed excellent electrocatalytic oxidation toward dopamine and uric acid with a large separation of peak potentials and a significant enhancement of peak currents. However, the electrochemical behavior of ascorbic acid may be depressed at the modified electrode. Differential pulse voltammetry was used for the simultaneous sensitive determination of dopamine and uric acid in the presence of excess ascorbic acid at this modified electrode. The current responses showed excellent linear relationships in the range of 2–30 µM and 9–100 µM for dopamine and uric acid, respectively. The detection limits were estimated to be 0.5 µM and 2.3 µM for dopamine and uric acid, respectively. In addition, this modified electrode showed excellent repeatability, good stability, and satisfactory reliability, thus indicating potential for the practical applications.     

Real-time detection of food-borne bacterial adenosine triphosphate (ATP) using dielectrophoretic force and a bioluminescence sensor

A copper hexacyanoferrate nanostructure was prepared on the surface of a disposable pencil graphite electrode. The resulting electrode exhibits an excellent electrocatalytic activity for the oxidation of L-cysteine. Cyclic voltammetry and chronoamperometry were employed to characterize the response to L-cysteine that changes linearly in the concentration range from 1 to 13 μM, with a detection limit of 0.13 μM (at an SNR of 3). Typical features of the sensor include low cost, simple preparation, fast response, good stability, selectivity, and reproducibility. It was applied to the determination of L-cysteine in urine.