Voltammetric determination of hydroxylamine in water samples using a 1-benzyl-4-ferrocenyl-1H-[1,2,3]-triazole/carbon nanotube-modified glassy carbon electrode

A modified glassy carbon electrode has been constructed using a 1-benzyl-4-ferrocenyl-1H-[1,2,3]-triazole along with multiwalled carbon nanotubes. The electrochemical behaviour of modified electrode has been investigated by cyclic voltammetry. Electrocatalytic activity of the modified electrode was investigated for the oxidation of hydroxylamine in 0.1 M phosphate-buffered solution of pH 8. The modified electrode showed electrocatalytic response to the oxidation of hydroxylamine at the potential of 330 mV. The linear range and detection limit for the detection of hydroxylamine in the optimum condition were found to be 4.0?×?10^?7 to 6.75?×?10^?4 M and 28.0?±?1.0 nM, respectively. Finally, the method was employed for the determination of hydroxylamine in water samples.     

Highly sensitive electrochemical detection of dopamine and uric acid on a novel carbon nanotube-modified ionic liquid-nanozeolite paste electrode

A novel biosensor has been constructed by incorporating modified nanosized natural zeolite and 3-hydroxypropanaminium acetate (HPAA) as a novel room temperature ionic liquid, supported on multiwalled carbon nanotube (MWCNTs) and employed for the simultaneous determination of dopamine (DA) and uric acid (UA). A detailed investigation by transmission electron microscopy and electrochemistry is performed in order to elucidate the preparation process and properties of the composites. The voltammetric studies using the modified carbon paste electrode show two well-resolved anodic peaks for DA and UA with a potential difference of 160 mV, revealing the possibility of the simultaneous electrochemical detection of these compounds. The modified carbon paste electrode shows good conductivity, stability, and extraction effect due to the synergic action of HPAA, MWCNTs, and iron ion-doped natrolite zeolite. Under optimized conditions, the peak currents are linear from 8.12?×?10^?7 to 3.01?×?10^?4?mol?L^?1 and from 9.31?×?10^?7 to 3.36?×?10^?4?mol?L^?1 with detection limits of 1.16?×?10^?7 and 1.33?×?10^?7?mol?L^?1 for DA and UA using the differential pulse voltammetric method, respectively. Finally, the modified carbon paste electrode proved to have good sensitivity and stability and is successfully applied for the simultaneous determination of DA and UA in human blood serum and urine samples.     

Benzoylferrocene-modified carbon nanotubes paste electrode as a voltammetric sensor for determination of hydrochlorothiazide in pharmaceutical and biological samples

The electrooxidation of hydrochlorothiazide (HCT) at the surface of a benzoylferrocene modified multi-walled carbon nanotube paste electrode was studied using electrochemical approaches. Under the optimized conditions (pH 7.0), the square wave voltammetric peak current of HCT increased linearly with HCT concentration in the ranges of 6.0?×?10^?7 to 3.0?×?10^?4 M. The detection limit was 9.0?×?10^?8 M HCT. The diffusion coefficient (D?=?1.75?×?10^?5 cm²/s) and electron transfer coefficient (α?=?0.45) for HCT oxidation were also determined. The proposed sensor was successfully applied for the determination of HCT in human urine and tablet samples.     

A selective sensor for nanolevel detection of lead (II) in hazardous wastes using ionic-liquid/Schiff base/MWCNTs/nanosilica as a highly sensitive composite

An effective potentiometric sensor had been fabricated for the rapid determination of Pb²⁺ based on carbon paste electrode consisting of room temperature ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate (BMIM-PF₆), multiwalled carbon nanotubes (MWCNTs), nanosilica, synthesized Schiff base, as an ionophore, and graphite powder. The constructed nanocomposite electrode showed better sensitivity, selectivity, response time, response stability, and lifetime in comparison with typical Pb²⁺ carbon paste electrode for the successfully determination of Pb²⁺ ions in water and in waste water samples. The best response for nanocomposite electrode was obtained with electrode composition of 18% ionophore, 20% BMIM-PF₆, 49% graphite powder, 10% MWCNT, and 3% nanosilica. The new electrode exhibited a Nernstian response (29.76?±?0.10 mV decade^?1) toward Pb²⁺ ions in the range of 5?×?10^?9?C1.0?×?10^?1 mol L^?1 with a detection limit of 2.51?×?10^?9 mol L^?1. The potentiometric response of prepared sensor is independent of the pH of test solution in the pH range of 4.5?C8.0. It has quick response with response time of about 6 s. The proposed electrode show fairly good selectivity over some alkali, alkaline earth, transition, and heavy metal ions.     

Sensitive and selective electrochemical sensor for magnolol based on the enhancement effect of multiwalled carbon nanotubes

Herein, insoluble multiwalled carbon nanotubes (MWNTs) were dispersed into N,N-dimethylformamide (DMF) via ultrasonication, resulting in a stable and homogeneous MWNTs suspension. After evaporation of DMF, the surface of glassy carbon electrode was successfully coated with MWNTs film, as confirmed from scanning electron microscopy measurements. In pH 7 phosphate buffer, an irreversible oxidation peak was observed for magnolol, and the peak currents greatly increased on MWNTs film surface. The influences of pH value, amount of MWNTs and accumulation conditions were studied. Based on the remarkable enhancement effect of MWNTs, a new electrochemical sensor with high sensitivity was developed for magnolol. The linear range was from 5 μg?L^?1 to 1 mg?L^?1, and the detection limit was 2 μg?L^?1 (7.51?×?10^?9?M) after a 3-min accumulation. This novel sensor was successfully used to detect the content of magnolol in Chinese traditional medicines, and the recovery was over the range from 98.1 to 99.1 %.     

Sensitive voltammetric determination of cysteamine using promazine hydrochloride as a mediator and modified multi-wall carbon nanotubes carbon paste electrodes

This paper presents a sensitive electrochemical method for the determination of cysteamine (CA) using promazine hydrochloride-modified multi-wall carbon nanotubes carbon paste electrode (PrH/MWCNTs CPE). Because of the good electrochemical activity of MWCNTs and the acceptable performance of promazine hydrochloride (PrH) as an electrocatalytic mediator, the modified electrode significantly enhanced the sensitivity for the detection of CA in comparison to the bare carbon paste electrode (CPE). All chemical parameters such as pH of solution, concentration of PrH and kinetic parameters of the system were investigated. Linear sweep voltammetric (LSV) method was used to follow the electrocatalytic effect of CA on the current–potential response of PrH. Under optimum conditions, the obtained net peak current ?I _p(I _sample???I _blank) was linear with CA concentrations in two dynamic ranges of 2.0–346.5 μmol l^?1 (?I _p?=?(0.0195?±?0.0043)C _CA?+?(0.7648?±?0.0397) (r ²?=?0.9948)) and 346.5–1,912.5 μmol l^?1 (?I _p?=?(0.0100?±?0.0026)C _CA?+?(3.8981?±?0.0828) (r ²?=?0.9911)) with a detection limit of 0.8 μmol l^?1. Finally, the PrH/MWCNTs CPE was successfully applied for the determination of CA in urine and drug samples with satisfactory results.     

Electrochemical and catalytic investigations of epinephrine,acetaminophen and folic acid at the surface of titanium dioxide nanoparticle-modified carbon paste electrode

In the present paper, the use of a carbon paste electrode modified with 1-(4-(1, 3-dithiolan-2-yl)-6, 7-dihydroxy-2-methyl-6, 7-dihydrobenzofuran-3-yl)ethanone (DDE) and TiO₂ nanoparticles prepared by a simple and rapid method was described. The modified electrode showed excellent properties for electrocatalytic oxidization of epinephrine (EP), acetaminophen (AC) and folic acid (FA). The apparent charge transfer rate constant, k _s?=?1.14 s^?1, and transfer coefficient, α?=?0.54, for electron transfer between the modifier and carbon paste electrode were calculated. It has been found that under optimum condition (pH?=?7.0) in cyclic voltammetry, the oxidation of EP occurs at a potential about 280 mV less positive than that of an unmodified carbon paste electrode. The values of transfer coefficients (α?=?0.46), catalytic rate constant (k?=?1.2?×?10⁴ M^?1 s^?1) and diffusion coefficient (D?=?2.70?×?10^?5 cm² s^?1) were calculated for EP. Differential pulse voltammetry (DPV) exhibited two linear dynamic ranges of 0.5 to 50.0 μM and 50.0 to 1,000 μM for EP. This modified electrode is quite effective not only for the detection of EP, AC and FA but also for the simultaneous determination of these species in a mixture. The limit of detection for EP, AC and FA is 0.10, 1.80 and 2.36 μM, respectively.     

Voltammetric sensor for simultaneous determination of ascorbic acid,acetaminophen, and tryptophan in pharmaceutical products

A novel carbon paste electrode modified with carbon nanotubes and 5-amino-2′-ethyl -biphenyl-2-ol was fabricated. The electrochemical study of the modified electrode, as well as its efficiency for electrocatalytic oxidation of ascorbic acid (AA), is described. The electrode was employed to study the electrocatalytic oxidation of AA, using cyclic voltammetry, chronoamperometry, and square-wave voltammetry (SWV) as diagnostic techniques. It has been found that the oxidation of AA at the surface of modified electrode occurs at a potential of about 250 mV less positive than that of an unmodified carbon paste electrode. SWV exhibits a linear dynamic range from 2.0?×?10^?7 to 5.0?×?10^?4 M and a detection limit of 1.0?×?10^?7 M for AA. In addition, this modified electrode was used for simultaneous determination of AA, acetaminophen (AC), and tryptophan (TRP). Finally, the modified electrode was used for determination of AA, AC, and TRP in pharmaceutical products.     

Enhanced electrocatalytic oxidation of hydroxylamine on Pt/polypyrrole composite modified glassy carbon electrode

A sensitive hydroxylamine sensor is developed by electrodeposition of Pt nanoparticles on pre-synthesized polypyrrole nanoparticles modified glassy carbon electrode. The modified electrode presents distinctly electrocatalytic activity toward hydroxylamine oxidation. The kinetic parameters such as the overall numbers of electrons involved in hydroxylamine oxidation, the electron transfer coefficient, standard heterogeneous rate constant, and diffusion coefficient are evaluated. The current response increases linearly with increasing hydroxylamine concentrations and exhibits two wide linear ranges of 5.0?×?10^?7–1.1?×?10^?3 and 1.1?×?10^?3–18.8?×?10^?3 M with a detection limit of 0.08 μM (s/n?=?3). The proposed electrode presents excellent operational and storage ability for determining hydroxylamine. Moreover, the sensor shows good sensitivity, selectivity, and reproducibility properties.     

Electrochemical methods for determination of thymine in medical pipefish samples based on HPMαFP/Ppy/GCE-modified electrode

A sensitive electrochemical method was developed for the voltammetric determination of thymine at a composite film-modified electrode 1-phenyl-3-methyl-4-(2-furoyl)-5-pyrazolone (HPMαFP)/polypyrrole (Ppy)/glassy carbon electrode (GCE). The electrochemical parameters of thymine were investigated by cyclic voltammetry and differential pulse voltammetry. In pH?=?7.4, one sensitive oxidation peak of thymine with E _pa?=?0.968 V was observed on the HPMαFP/PPy-modified electrode. The difference of peak potential (?E _pa) was 188 mV lower than that for bare GCE. Compared to the bare GCE and Ppy/GCE, the HPMαFP/Ppy/GCE-modified electrode showed an excellent electrocatalytic effect on the oxidation of thymine and displayed a shift of the oxidation potential in the negative direction with significant increase in the peak current. Under the optimum condition, the concentration calibration range and detection limit are 2?×?10^?6–1?×?10^?4 and 4.85?×?10^?7?M for thymine. This developed method had been applied to the direct determination of thymine in medical pipefish samples with satisfactory results.     

Synthesis,Spectral Characterization,DNA Binding Studies and Antimicrobial Activity of Co(II), Ni(II), Zn(II), Fe(III) and VO(IV) Complexes with 4-Aminoantipyrine Schiff Base of Ortho-Vanillin

A series of transition metal complexes of Co(II), Ni(II), Zn(II), Fe(III) and VO(IV) have been synthesized involving the Schiff base, 2,3-dimethyl-1-phenyl-4-(2-hydroxy-3-methoxy benzylideneamino)-pyrazol-5-one(L), obtained by condensation of 4-aminoantipyrine with 3-methoxy salicylaldehyde. Structural features were obtained from their FT-IR, UV–vis, NMR, ESI Mass, elemental analysis, magnetic moments, molar conductivity and thermal analysis studies. The Schiff base acts as a monovalent bidentate ligand, coordinating through the azomethine nitrogen and phenolic oxygen atom. Based on elemental and spectral studies six coordinated geometry is assigned to Co(II), Ni(II), Fe(III) and VO(IV) complexes and four coordinated geometry is assigned to Zn(II) complex. The interaction of metal complexes with Calf thymus DNA were carried out by UV–VIS titrations, fluorescence spectroscopy and viscosity measurements. The binding constants (K_b) of the complexes were determined as 5?×?10⁵ M^?1 for Co(II) complex, 1.33?×?10⁴ M^?1 for Ni(II) complex, 3.33?×?10⁵ M^?1 for Zn(II) complex, 1.25?×?10⁵ M^?1 for Fe(III) complex and 8?×?10⁵ M^?1 for VO(IV) complex. Quenching studies of the complexes indicate that these complexes strongly bind to DNA. Viscosity measurements indicate the binding mode of complexes with CT DNA by intercalation through groove. The ligand and it’s metal complexes were screened for their antimicrobial activity against bacteria. The results showed the metal complexes to be biologically active, while the ligand to be inactive.     

X-ray structure refinement and ionic conductivity of Na6.69Ca3.355(SO4)6Cl0.77F0.63

The structure of Na_6.69Ca_3.355(SO₄)₆Cl_0.77F_0.63, isostructural with fluorapatite, was determined by X-ray powder diffraction methods. The results of Rietveld refinement revealed a space group P6₃/m with lattice parameters of a?=?9.477 (2) Å, c?=?6.865 (5) Å. Final refinement led to R _F?=?1.83 % and R _B?=?7.64 %. The location of Na⁺ ions in the M (2) sites surrounding the channels was related particularly to the high polarizability of the Ca²⁺. The ionic conductivity over a wide range of temperature was investigated according to the complex impedance method. The highest overall conductivity values were found at σ _500 °C?=?1.03?×?10^?5?S?cm^?1 and E_a?=?0.70 eV.     

Multiwalled carbon nanotubes decorated with nitrogen, palladium co-doped TiO2 (MWCNT/N, Pd co-doped TiO2) for visible light photocatalytic degradation of Eosin Yellow in water

Multiwalled carbon nanotube (MWCNT/N), Pd co-doped TiO₂ nanocomposites were prepared by calcining the hydrolysis products of the reaction of titanium isopropoxide, Ti(OC₃H₇)₄ containing multiwalled carbon nanotubes with aqueous ammonia. The prepared samples were characterised by Fourier transform infrared spectroscopy, Raman spectroscopy, thermogravimetric analysis, diffuse reflectance UV?CVis spectrophotometry (DRUV?CVis), XRD, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). DRUV?CVis analysis confirmed the red shift in the absorption edge at lower MWCNT percentages. SEM and TEM images showed the complete coverage of the MWCNTs with clusters of anatase TiO₂ at low MWCNT percentages. Higher MWCNT levels led to their aggregation and consequently poor coverage by N, Pd co-doped TiO₂. The photocatalytic activities of the nanocomposites were monitored by photodegradation of Eosin Yellow under simulated solar and visible light irradiation (???>?450?nm). Irradiation with simulated solar radiation gave higher dye-degradation rates compared to visible radiation. The optimum MWCNT weight percentage in the composites was found to be 0.5. High degradation-rate constants of 3.42?×?10^?2 and 5.18?×?10^?3?min^?1 were realised for the 0.5% MWCNT/N, Pd co-doped TiO₂ composite, using simulated solar light and visible light, respectively.     

Effect of doping functionalized MWCNTs on the electrochemical performances of Li<Subscript>2</Subscript>CoSiO<Subscript>4</Subscript> for lithium-ion batteries

We report the synthesis of Li₂CoSiO₄ by the sol-gel method and the preparation of a composite electrode by incorporating functionalized multi-walled carbon nanotubes (fn. MWCNTs) as conductive additive. XRD pattern of the composite confirms the structural stability of Li₂CoSiO₄ even after the addition of fn. MWCNTs. SEM images of the composite reveal the presence of conductive bridges formed by MWCNTs between the submicron-sized particles of Li₂CoSiO₄. The cyclic voltammograms of the composite cathode show redox peaks with higher current density than pure Li₂CoSiO₄ and the current density increases with increase in sweep rate. The diffusion coefficient of lithium has been improved by the addition of fn. MWCNTs from 1 × 10^?14 to 8 × 10^?14 cm²/s as calculated using Randles-Sevcik equation. The charge-discharge cycling performance of both pure Li₂CoSiO₄ and composite cathode has been discussed.     

Colorimetric detection of melamine based on <Emphasis Type="Italic">p</Emphasis>-chlorobenzenesulfonic acid-modified AuNPs

A highly selective and sensitive method is developed for colorimetric detection of melamine using gold nanoparticles (AuNPs) functionalized with p-chlorobenzenesulfonic acid. The addition of melamine induced the aggregation of AuNPs, as evidenced from the morphological characterizations and the color changed from red wine to blue, which could also be monitored by the UV–visible spectrometer and even naked eyes. This process caused a significant increase in the absorbance ratio (A_650nm/A_520nm) of p-chlorobenzenesulfonic acid–AuNPs. Under optimized conditions, the system exhibited a linear response to melamine in the range of 6.0 × 10^?7–1.5 × 10^?6 mol L^?1 with a correlation coefficient of 0.997, and the limit of detection can even be 2.3 nM, which was much lower than some other methods and the safe limits (20 μM in both the USA and EU, 8.0 μM for infant formula in China, 1.2 μM in the CAC (Codex Alimentarius Commission) review for melamine in liquid infant formula). More importantly, the developed method presented excellent tolerance to coexisting common metal ions such as Ca²⁺, Zn²⁺, whose concentration is 1000 times of melamine, so that it had been applied to the analysis of melamine in liquid milk and milk powder with the recovery of 97.0–101 % and 100–103 %, respectively, indicating that the proposed method is quite a highly effective means to determine melamine in milk products.     

Selective Fluorescence Sensing of Deoxycytidine 5��-Monophosphate (dCMP) Employing a Bis(diphenylphosphate)diimine Ligand

A new bis(diphenylphosphate)diimine ligand (BP1) was prepared and evaluated for its ability for selective detection of deoxycytidine 5??-monophosphate (dCMP). BP1 exhibited off-type fluorescence in the presence of dCMP. The fluorescence of BP1 was significantly quenched upon the addition of 2.5?×?10^?4 M dCMP and the detection limit was 1.25?×?10^?5 M in MeCN-H₂O (1:1, v/v). The binding ratio between BP1 and dCMP was determined to be 1:1 with the binding constant of 3.98?±?0.60?×?10^?3 M^?1.     

The first electrochemical sensor for determination of mangiferin based on an ionic liquid–graphene nanosheets paste electrode

A novel carbon paste electrode modified with graphene nanosheets and an ionic liquid (n-hexyl-3-methylimidazolium hexafluoro phosphate) was fabricated and used for the electrochemical study of mangiferin for the first time. This modified electrode offers a considerable improvement in voltammetric sensitivity toward mangiferin, compared to the bare electrode. Square wave voltammetry (SWV) exhibits a linear dynamic range from 5.0?×?10^?8 to 2.0?×?10^?4 M and a detection limit of 20.0 nM for mangiferin. Finally, the proposed method was successfully applied to the determination of mangiferin in real samples such as serum and urine.     

Nitrogen-doped multi-walled carbon nanotubes for paracetamol sensing

A novel sensor consisting of nitrogen-doped multi-walled carbon nanotubes was fabricated by means of chemical vapor deposition technique with decomposition of acetonitrile onto oxidized silicon wafer using ferrocene as catalyst. The electrochemical response of carbon nanotubes-based sensor towards oxidation of paracetamol to N-acetyl-p-quinone imine was investigated in phosphate buffer solution (pH 7.0) by means of standard electrochemical techniques. A quasi-reversible response for oxidation of paracetamol was identified on carbon nanotubes-based sensor with detection limit and sensitivity of 0.485 μM and 0.8406 A M^?1 cm^?2, respectively. It was found that the nitrogen doping in carbon nanotubes enhances the sensor's detection ability. Namely, electrochemical studies performed on film consisting of pristine carbon nanotubes reveal as well quasi-reversible response towards oxidation of paracetamol but nevertheless poorer detection ability and sensitivity (0.950 μM; 0.601 A M^?1 cm^?2). The findings strongly suggest the application of nitrogen-doped carbon nanotubes in biosensing.     

Determination of the Thermal Expansion Coefficient of Single-Wall Carbon Nanotubes by Raman Spectroscopy

We have examined the effect of high temperature on single-wall carbon nanotubes under air and nitrogen ambient by Raman spectroscopy. We observe the temperature dependence of the radial breathing mode and the G-band modes. The thermal expansion coefficient (β) of the bundled nanotubes is obtained experimentally using the estimated volume from Raman scattering. β behaves linearly with temperature from 0.33 × 10^?5 K^?1 to 0.28 × 10^?5 K^?1 in air and from 0.58 × 10^?5 K^?1 to 0.47 × 10^?5 K^?1 in nitrogen ambient, respectively. The temperature dependence of the radial breathing mode Raman frequencies is consistent with a pure temperature effect.     

A calix[4]arene derivative-doped perchlorate-selective membrane electrodes with/without multi-walled carbon nanotubes

In this study, poly (vinyl chloride)(PVC) membrane electrodes with/without multi-walled carbon nanotubes (MWCNTs) based on a calix[4]arene derivative for perchlorate ion were described. The influence of membrane composition, pH, conditioning solution on the potentiometric response of the electrodes was investigated. Perchlorate-selective PVC membrane electrode exhibited a slope of 47.8 ± 0.6 mV/pClO₄ in the range of 1.0 × 10^?7–1.0 × 10^?1 mol L^?1at pH 4.0 while the coated Pt electrodes with MWCNT-OH, MWCNT-COOH and MWCNT displayed slopes of 46.1 ± 0.7 mV/pClO₄ (5.0 × 10^?6–1.0 × 10^?1 mol L^?1), 50.4 ± 1.9 mV/pClO₄ (1.0 × 10^?6–1.0 × 10^?1 mol L^?1) and 44.4 ± 0.3 mV/pClO₄ (1.0 × 10^?5–1.0 × 10^?1 mol L^?1), respectively. Other response characteristics of these electrodes such as response time, lifetime and detection limit were identified, and the selectivity coefficients towards various anions were calculated by separate solution method. Moreover, the perchlorate-selective electrodes described here were successfully used as an indicator electrode for the determination of perchlorate in real samples such as tap water, river water and human urine by direct calibration method.