A novel nitrite sensor based on graphene/polypyrrole/chitosan nanocomposite modified glassy carbon electrode

A novel nitrite sensor was fabricated based on a graphene/polypyrrole/chitosan nanocomposite film modified glassy carbon electrode. The nanocomposite film was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. The electron transfer behaviour of the modified electrodes was investigated in [Fe(CN)(6)](3-)/(4-) redox probe using cyclic voltammetry and electrochemical impedance spectroscopy. Differential pulse voltammetry and amperometry were used to study the electrochemical properties of the proposed sensor. Under optimum conditions, the sensor exhibited good reproducibility and stability for nitrite determination. Linear response was obtained in the range of 0.5-722 μM with a detection limit of 0.1 μM (S/N = 3) for nitrite determination.     

Development of an amperometric sulfite biosensor based on a gold nanoparticles/chitosan/multiwalled carbon nanotubes/polyaniline-modified gold electrode

A sulfite oxidase (SOx) purified from leaves of Syzygium cumini (Jamun) was immobilized covalently onto a gold nanoparticles (AuNPs)/chitosan (CHIT)/carboxylated multiwalled carbon nanotubes (cMWCNTs)/polyaniline (PANI) composite that was electrodeposited onto the surface of a gold (Au) electrode. A novel and highly sensitive sulfite biosensor was developed that used this enzyme electrode (SOx/AuNPs/CHIT/cMWCNT/PANI/Au) as the working electrode, Ag/AgCl as the standard electrode, and Pt wire as the auxiliary electrode. The modified electrode was characterized by Fourier transform infrared (FTIR) spectroscopy, cyclic voltammetry (CV), scanning electron microscopy (SEM), and electrochemical impedance spectroscopy (EIS) before and after the immobilization of the SOx. The sensor produced its optimum response within 3 s when operated at 50 mVs⁻¹ in 0.1 M phosphate buffer, pH 7.0, and at 35 °C. The linear range and detection limit of the sensor were 0.75–400 μM and 0.5 μM (S/N = 3), respectively. The biosensor was employed to determine sulfite levels in fruit juices and alcoholic beverages. The enzyme electrode was used 300 times over a period of three months when stored at 4 °C.     

LaNi<Subscript>0.5</Subscript>Ti<Subscript>0.5</Subscript>O<Subscript>3</Subscript>/CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript>-based sensor for sensitive determination of paracetamol

A novel electrochemical sensor based on LaNi_0.5Ti_0.5O₃/CoFe₂O₄ nanoparticle-modified electrode (LNT–CFO/GCE) for sensitive determination of paracetamol (PAR) was presented. Experimental conditions such as the concentration of LNT–CFO, pH value, and applied potential were investigated. Under the optimum conditions, the electrochemical performances of LNT–CFO/GCE have been researched on the oxidation of PAR. The electrochemical behaviors of PAR on LNT–CFO/GCE were investigated by cyclic voltammetry. The results showed that LNT–CFO/GCE exhibited excellent promotion to the oxidation of PAR. The over-potential of PAR decreased significantly on the modified electrode compared with that on bare GCE. Furthermore, the sensor exhibits good reproducibility, stability, and selectivity in PAR determination. Linear response was obtained in the range of 0.5 to 901 μM with a detection limit of 0.19 μM for PAR.     

Determination of Nitrite by a Modified Electrode of Poly(1-Naphthylamine) Film Doped with Dawson-Type Heteropolyanions

 The voltammetric behavior of the electrode modified with poly(1-naphthylamine) film doped with α-P₂W₁₈ heteropolyanions was investigated. The concentration of the modifier, the acidity of the medium and the scan range of potential had obvious effects on the electrochemical characteristics of the electrode. The electrocatalytical characteristics of the film electrode were studied by cyclic voltammetry and other methods. It is suggested that the electrocatalytic reaction of nitrite is controlled by its diffusion. The applicability of the electrode was assessed by the determination of nitrite in waste-water. Determination limit for nitrite was 5 × 10⁻⁷ mol.L⁻¹. Received August 23, 1999. Revision January 2, 2001     

High sensitive determination of trace amount of cobalt by catalytic adsorptive stripping voltammetry

A very sensitive and selective catalytic adsorptive cathodic stripping procedure for trace measurements of cobalt is presented. The method is based on adsorptive accumulation of cobalt-CCA (calcon carboxylic acid) complex onto a hanging mercury drop electrode followed by reduction of the adsorbed species by voltammetric scan using differential pulse modulation. The reduction current is enhanced catalytically by nitrite. The effect of various parameters such as pH, concentration of CCA, concentration of nitrite, accumulation potential and accumulation time on the selectivity and sensitivity were studied. The optimum condition for the analysis of cobalt, include pH 5.2 (Acetate buffer), 2.1 μM clacon carboxylic acid, 0.032 M sodium nitrite and an accumulation potential of 0.05 V (versus Ag/AgCl). Under these optimum conditions and for an accumulation time of 60 s, the measured peak current at −0.480 V is proportional to the concentration of cobalt over the entire concentration range tested 0.003–2.0 ng ml⁻¹ with a detection limit of 1 pg ml⁻¹ for an accumulation time of 60 s and 2.0–10.0 ng ml⁻¹ for an accumulation time of 40 s. The relative standard deviations for ten replicate measurement of 0.5 ng ml⁻¹ of cobalt were 3.1%. The main advantage of this new system is the microtrace Co(II) determination by ASV. The method was applied to determination of cobalt in a water sample and some analytical grade salts with satisfactory results. Published in Elektrokhimiya in Russian, 2009, Vol. 45, No. 2, pp. 221–228. The article is published in the original.     

浊点萃取-分光光度法测定痕量NO2-

建立了浊点萃取-分光光度法测定痕量NO2-根的方法.以对氨基苯磺酸和α-萘胺为络合剂,非离子型表面活性剂TritonX-100为萃取剂,富集、分离水样中痕量NO2-,采用可见吸收光谱法进行检测.研究了溶液的酸度、试剂用量、平衡时间、平衡温度、干扰离子对浊点萃取效果的影响,并得到最佳实验条件:5％的TritonX-100用量2.0mL、平衡温度85℃、平衡时间10min、对氨基苯磺酸和α-萘胺均为0.3mL、0.1mol/LH2SO4溶液0.5mL.在最佳实验条件下,对氨基苯磺酸、α-萘胺和NO2-生成的络合物被萃取到TritonX-100表面活性剂相并与水相分开.该方法适用于环境水样中痕量NO2-的测定.     

Chemically functionalized glassy carbon spheres: a new covalent bulk modified composite electrode for the simultaneous determination of lead and cadmium

A new type of covalent bulk modified glassy carbon composite electrode has been fabricated and utilized in the simultaneous determination of lead and cadmium ions in aqueous medium. The covalent bulk modification was achieved by the chemical reduction of 2-hydroxybenzoic acid diazonium tetrafluroborate in the presence of hypophosphorous acid as a chemical reducing agent. The covalent attachment of the modifier molecule was examined by studying Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and the surface morphology was examined by scanning electron microscopy images. The electrochemistry of modified glassy carbon spheres was studied by its cyclic voltammetry to decipher the complexing ability of the modifier molecules towards Pb²⁺ and Cd²⁺ ions. The developed sensor showed a linear response in the concentration range 1–10 μM with a detection limit of 0.18 and 0.20 μM for lead and cadmium, respectively. The applicability of the proposed sensor has been checked by measuring the lead and cadmium levels quantitatively from sewage water and battery effluent samples.     

Immobilization of nickel-dipicolinic acid onto a glassy carbon electrode modified with bimetallic Au-Pt inorganic-organic hybrid nanocomposite: Application to micromolar detection of fructose

This work describes the electrochemical behavior of nickel-dipicolinic acid (Ni-DPA) film immobilized on the surface of bimetallic Au-Pt inorganic-organic hybrid nanocomposite glassy carbon electrode and its electrocatalytic activity toward the oxidation of fructose. The electrode possesses a three-dimensional (3D) porous network nano architecture, in which the bimetallic Au-Pt serving as metal nano-particle based microelectrode ensembles are distributed in the matrix of interlaced 3,3′,5,5′-tetramethylbenzidine (TMB) organic nanofibers (NFs). The surface structure and composition of the sensor was characterized by scanning electron microscopy (SEM). Electrocatalytic oxidation of fructose on the surface of modified electrode was investigated with cyclic voltammetry and chronoamperometry methods and the results show that the Ni-DPA film displays excellent electrochemical catalytic activities towards fructose oxidation. The hydrodynamic amperometry at rotating modified electrode at constant potential versus reference electrode was used for detection of fructose. Under optimized conditions the calibration plots are linear in the concentration range 0.5 to 70 μM and detection limit was found to be 0.1 μM.     

Electrochemical determination of nitrite via covalent immobilization of a single-walled carbon nanotubes and single stranded deoxyribonucleic acid nanocomposite on a glassy carbon electrode

A novel method has been developed for determination of nitrite by modifying the surface of a glassy carbon electrode (GCE) using single-walled carbon nanotubes with covalently immobilized single-strand deoxyribonucleic acid. The modified electrodes were characterized by field emission scanning electron microscopy, X-ray photoelectron spectroscopy, and electrochemical techniques. The results demonstrate that the nanotube-DNA nanocomposite has been successfully immobilized on the surface of the GCE. The new electrode, under optimum conditions at room temperature, exhibits excellent electrocatalytic activity towards the oxidation of nitrite, with a significantly reduction of the overpotential. The linear range for the detection of nitrite is from 0.6 to 540 μM, with a sensitivity of 0.216 μA?μM^?1, and a detection limit as low as 0.15 μM. The electrode showed good reproducibility and high stability and was successfully used to analyze nitrite in water and sausage samples.     

Selective determination of dopamine with a cibacron blue/poly-1,5-diaminonaphthalene composite film

A selective detection method for dopamine (DA) was developed by incorporating cibacron blue (F3GA) into poly-1,5-diaminonaphthalene (PDAN) layer. Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry (CV) were employed to characterize the modified surfaces. The modified electrode was effective in selectively facilitating the electron transfer of DA and blocking the interferences of negatively charged species attributed to the sulfonate groups in the F3GA/PDAN composite film. This method enabled the determination of DA in the presence of various interfering species, including ascorbic acid (AA), in a phosphate buffer solution (pH 7.4). The modified electrode demonstrated good performance in the detection of DA in a concentration range of 5.0-100 μM, with a detection limit (k = 3) of 0.1 ± 0.01 μM. The application was conducted for the determination of DA in a human urine sample and the sensor was proven to be rapid, has excellent selectivity, and stable amperometric response.     

A silver optical sensor based on 5(p-dimethylaminobenzylidene)rhodanine immobilized on a triacetylcellulose membrane

An optical sensor has been proposed for the determination of silver by spectrophotometry. The sensor was prepared by immobilizing 5(p-dimethylaminobenzylidene)rhodanine on a transparent triacetylcellulose membrane. The effect of different variables on the response of the sensor was studied and the optimum conditions were established. The sensor responded linearly in the range 1.8–55.6 μM of silver with a limit of detection of 0.8 μM and a response time range of 8–10 min depending on the concentration of the silver ions. The presented optode is reversible and stable if stored in water for more than one month without reagent leaching. The relative standard deviation for seven replicated measurement of 4.6 and 37 μM silver was 3.15 and 2.76%, respectively. The sensor was successfully applied to the determination of silver in a silver sulphadiazine cream, an ore sample, and a radiology film. The text was submitted by the authors in English.     

Development of an Innovative Nitrite Sensing Platform Based on the Construction of an Electrochemical Composite Sensor of Polymer Coated CNTs and Decorated with Magnetite Nanoparticles

Electrochemical determination of nitrite in real water samples is achieved using simple and efficient electrochemical sensor. The sensor is fabricated by electrodeposition of a thin layer of poly(3,4-ethylenedioxythiophene) sandwiched by drop-casting two thin layers of CNTs and iron oxide nanoparticles (Fe₃O₄) over a GC electrode surface. Voltammetry determination of nitrite in tap water and wastewater samples in the concentration range (0.5–150 μM) is successfully achieved with detection limits of 22 and 24 nM, respectively. Practical application of the GC/CNT/PEDOT/Fe₃O₄ sensor is efficiently assessed in real water samples for nitrite determination with acceptable recoveries, excellent anti-interference ability and long-term stability.     

Functionalization of platinum nanoparticles for electrochemical detection of nitrite

In this work, a novel electrochemical method for nitrite detection by using functionalized platinum nanoparticles (PtNPs) is proposed. Firstly, a gold electrode is immobilized with 4-(2-aminoethyl)benzenamine. Then, PtNPs are modified with 5-[1, 2]dithiolan-3-yl-pentanoic acid [2-(naphthalene-1-ylamino)-ethyl]amide (DPAN). Consequently, in the presence of nitrite ions, Griess reaction occurs between 4-(2-aminoethyl)benzenamine on the electrode and DPAN on PtNPs, thus PtNPs are localized onto the electrode surface. So, PtNPs-electrocatalyzed reduction of H₂O₂ can be achieved to correlate the electrochemical signal with the concentration of nitrite ions. The linear concentration range can be as wide as 10–1,000 μM, while the detection limit is as low as 5 μM. The proposed method has been also successfully applied to the detection of nitrite with the local lake water, and the result is well consistent with that obtained by UV-visible spectrophotometric method. So, this method has potential use for monitoring nitrite in drinking water supplies in the future.     

A Sensitive and Selective Nitrite Detection in Water Using Graphene/Platinum Nanocomposite

A glassy carbon electrode modified with reduced graphene oxide and platinum nanocomposite film was developed simply by electrochemical method for the sensitive and selective detection of nitrite in water. The electrochemical reduction of graphene oxide (GO) efficiently eliminates oxygen‐containing functional groups. Pt nanoparticles were electrochemically and homogeneously deposited on the ErGO surface. Field emission scanning electron microscopy (FE‐SEM), Raman spectroscopy, attenuated total reflectance‐fourier transform infrared spectroscopy (ATR‐FTIR), electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV) were used to examine the surface morphology and electrocatalytic properties of the Pt‐ErGO nanocomposite film‐modified electrode surface. The fabricated nitrite sensor showed good electrochemical performance with two linear ranges; one from 5 to 100 µM (R²=0.9995) and the other from 100 to 1000 µM (R²=0.9972) and a detection limit of 0.22 µM. The proposed sensor was successfully applied for the detection of nitrite in tap water samples which proves performance of the Pt‐ErGO nanocomposite films.     

Electrochemical oxidation of salicylic acid at well-aligned multiwalled carbon nanotube electrode and its detection

In this paper, an electrochemical sensor for sensitive and convenient determination of salicylic acid (SA) was constructed using well-aligned multiwalled carbon nanotubes as electrode material. Compared to the glassy carbon electrode, the electro-oxidation of SA significantly enhanced at the multiwalled carbon nanotube (MWCNT) electrode. The MWCNT electrode shows a sensitivity of 59.25 μA mM⁻¹, a low detection limit of 0.8 × 10⁻⁶ M and a good response linear range with SA concentration from 2.0 × 10⁻⁶ to 3.0 × 10⁻³ M. In addition, acetylsalicylic acid was determined indirectly after hydrolysis to SA and acetic acid, which simplified the detection process. The mechanism of electrochemical oxidation of SA at the MWCNT electrode is also discussed.     

A highly selective and sensitive dopamine and uric acid biosensor fabricated with functionalized ordered mesoporous carbon and hydrophobic ionic liquid

An ordered mesoporous carbon material functionalized with carboxylic acid groups was synthesized. It was characterized by powder X-ray diffraction, transmission electron microscopy, Fourier transform IR spectroscopy and N₂ adsorption/desorption. Furthermore, this material was used to modify an electrode surface combined with a hydrophobic ionic liquid. The functionalized ordered mesoporous carbon/ionic liquid gel modified electrode shows excellent electrocatalytic performances for the oxidation of dopamine, uric acid and ascorbic acid. The presence of the ionic liquid promotes the electron transfer. Linear responses for dopamine and uric acid were obtained in the ranges of 0.1 to 500 μM and from 0.1 to 100 μM with detection limits of 4.1 and 2.5 nM (signal-to-noise ratio of 3), respectively, under optimum conditions. A quick and sensitive biosensor based on functionalized ordered mesoporous carbon and an ionic liquid has been developed for the first time for the detection of dopamine and uric acid in the presence of a large amount of ascorbic acid.     

Simultaneous electrochemical determination of nitrate and nitrite in aqueous solution using Ag-doped zeolite-expanded graphite-epoxy electrode

In this work a new electrochemical sensor based on an Ag-doped zeolite-expanded graphite-epoxy composite electrode (AgZEGE) was evaluated as a novel alternative for the simultaneous quantitative determination of nitrate and nitrite in aqueous solutions. Cyclic voltammetry was used to characterize the electrochemical behavior of the electrode in the presence of individual or mixtures of nitrate and nitrite anions in 0.1 M Na₂SO₄ supporting electrolyte. Linear dependences of current versus nitrate and nitrite concentrations were obtained for the concentration ranges of 1-10 mM for nitrate and 0.1-1 mM for nitrite using cyclic voltammetry (CV), chronoamperometry (CA), and multiple-pulsed amperometry (MPA) procedures. The comparative assessment of the electrochemical behavior of the individual anions and mixtures of anions on this modified electrode allowed determining the working conditions for the simultaneous detection of the nitrite and nitrate anions. Applying MPA allowed enhancement of the sensitivity for direct and indirect nitrate detection and also for nitrite detection. The proposed sensor was applied in tap water samples spiked with known nitrate and nitrite concentrations and the results were in agreement with those obtained by a comparative spectrophotometric method. This work demonstrates that using multiple-pulse amperometry with the Ag-doped zeolite-expanded graphite-epoxy composite electrode provides a real opportunity for the simultaneous detection of nitrite and nitrate in aqueous solutions.     

Electrochemical sensor for Baicalein using a carbon paste electrode doped with carbon nanotubes

We report on the voltammetric determination of the flavonoid Baicalein by using a carbon paste electrode that was doped with multi-walled carbon nanotubes. The resulting sensor exhibits excellent redox activity towards Baicalein due to the large surface area and good conductivity of the electrode. Cyclic voltammetry at various scan rates was used to investigate the redox properties of Baicalein. At the optimum conditions, the sensor displays a linear current response to Baicalein in the 0.02–10 μM concentration range, with a limit of detection of 4.2 n M. The method was successfully applied to the determination of Baicalein in spiked human blood serum samples and in a Chinese oral liquid.

Layer-by-layer sensor architecture of polymers and nanoparticles for electrochemical detection of uric acid in human urine samples

Excessive uric acid levels in the human body (hyperuricemia) are the main causes of kidney stones and diabetes. In this study, a layer-by-layer arrangement of polymers and nanocomposites is used as a new electrode sensing material for rapid and direct electrochemical determination of uric acid (UA). The electrode surface architecture was constructed by the incorporation of poly (amidoamine) dendrimer with 0.5 generation (poly (amidoamine) [PAMAM] [D-G0.5]) of multiwalled carbon nanotube-silver nanoparticles (MWCNT-AgNP) and a poly (neutral-red) (poly [NR]) polymer. The PAMAM (D-G0.5)/MWCNT-AgNP/poly (NR)-coated electrode has a good electrocatalytic activity for the determination of UA using cyclic voltammetry and showed remarkable enhancement in current response at a low-oxidation potential (0.3 V). Under optimal conditions, the developed electrochemical sensor showed an excellent and wide linear range for the determination of UA (i.e. 0.016 μM–2500 μM), and the limit of detection was found to be 0.005 μM. The modified sensor system demonstrated excellent sensitivity and selectivity toward the detection of UA in the presence of interfering substances, which are commonly found in urine and human fluid samples. Furthermore, the developed sensor has represented both reproducibility and excellent stability for the UA determination in real samples (human urine).     

Multi-wall carbon nanotubes and TiO2 as a sensor for electrocatalytic determination of epinephrinein the presence of p-chloranil as a mediator

In this work, we describe an electrochemical method using p-chloranil as a mediator and multi-wall carbon nanotube and TiO₂ as sensors for sensitive determination of epinephrine (EP) in aqueous solution at pH = 10.0. It has been found that under optimum condition (pH 10.0) in cyclic voltammetry, the oxidation of EP occurred at a potential about 171 mV less positive than that unmodified carbon nanotube paste electrode. The diffusion coefficient (D) and the kinetic parameters, such as electron transfer coefficient, (α) and heterogeneous rate constant (k _h) for EP were also determined using electrochemical approaches. The electrocatalytic currents increase linearly with the EP concentration over the range 0.6–135 μM. The detection limits for EP will be equal to 0.25 μM. The relative standard deviation percentage values for 10.0 and 15.0 μM EP were 1.7% and 1.9%, respectively. Finally, this modified electrode was also examined as a selective, simple, and precise new electrochemical sensor for the determination of EP in real sample such as urine and epinephrine injection solution.