296 resultados para CLAY-MODIFIED ELECTRODES

em Indian Institute of Science - Bangalore - Índia


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Polyaniline (PANI) is one of the most extensively used conjugated polymers in the design of electrochemical sensors. In this study, we report electrochemical dye detection based on PANI for the adsorption of both anionic and cationic dyes from solution. The inherent property of PANI to adsorb dyes has been explored for the development of electrochemical detection of dye in solution. The PANI film was grown on electrode via electrochemical polymerization. The as grown PANI film could easily adsorb the dye in the electrolyte solution and form an insulating layer on the PANI coated electrode. As a result, the current intensity of the PANI film was significantly altered. Furthermore, PANI coated stainless steel (SS) electrodes show a change in the current intensity of Fe2+/Fe3+ redox peaks due to the addition of dye in electrolyte solution. PANI films coated on both Pt electrodes and non-expensive SS electrodes showed the concentration of dye adsorbed is directly proportional to the current intensity or potential shift and thus can be used for the quantitative detection of textile dyes at very low concentrations. (C) 2011 Elsevier B.V. All rights reserved.

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Donor-acceptor-donor-structured thiophene derivative-based conducting polymer poly(7,9-dithiophene-2yl-8H-cyclopentaa]acenaphthalene-8-one) was chemically synthesized. This polymer was used to modify both glassy-carbon and carbon-paste electrode, which was used to detect lead(II) ions present in water in the range of 1 mM to 0.1 mu M. Cyclic voltammetry confirms the formation of the co-ordination complex between the soft segment of polymer and the dissolved lead ion. Anodic stripping voltammetry was carried out by the modified electrode to determine the lower limit of detection of dissolved lead(II) species in the solution. Differential adsorptive stripping and impedance measurements were also conducted to find the lowest possible response of the as-synthesized polymer to lead(II) ion in water. The electrochemical performance of the modified electrodes at different pH (4, 7 and 9) environments was carried out by stripping voltammetry, to get optimum sensitivity and stability under these conditions. Finally, interference analysis was carried out to detect the modified electrode's sensitivity towards lead ion affinity in water.

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The electrochemical profiles of exfoliated graphite electrodes (EG) and glassy carbon electrodes (GCE) were recorded using cyclic voltammetry and square wave voltammetry in the presence of various supporting electrolytes and Fe(CN)(6)](3-/4-), Ru(NH3)(6)](2+/3+), ferrocene redox probes. In the supporting electrolytes (KCl, H2SO4, NaOH, tetrabutylammoniumtetraflouroborate, phosphate buffers), the potential windows of EG were found in some cases to be about 200 mV larger than that of GCE. The electroactive surface area of EG was estimated to be 19.5 % larger than the GCE which resulted in higher peak currents on the EG electrode. Furthermore, EG was modified with various nanomaterials such as poly (propylene imine) dendrimer, gold nanoparticles, and dendrimer-gold nanoparticles composite. The morphologies of the modified electrodes were studied using scanning electron microscopy and their electrochemical reactivities in the three redox probes were investigated. The current and the reversibility of redox probes were enhanced with the presence of modifiers in different degrees with dendrimer and gold nanoparticles having a favorable edge.

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An alternative antibody-free strategy for the rapid electrochemical detection of cardiac myoglobin has been demonstrated here using hydrothermally synthesized TiO2 nanotubes (Ti-NT). The denaturant induced unfolding of myoglobin led to easy access of the deeply buried electroactive heme center and thus the efficient reversible electron transfer from protein to electrode surface. The sensing performance of the Ti-NT modified electrodes were compared vis a vis commercially available titania and GCEs. The tubular morphology of the Ti-NT led to facile transfer of electrons to the electrode surface, which eventually provided a linear current response (obtained from cyclic voltammetry) over a wide range of Mb concentration. The sensitivity of the Ti-NT based sensor was remarkable and was equal to 18 mu A mg(-1) ml (detection limit = 50 nM). This coupled with the rapid analysis time of a few tens of minutes (compared to a few days for ELISA) demonstrates its potential usefulness for the early detection of acute myocardial infarction (AMI).

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Modification of exfoliated graphite (EG) electrode with generation 2 poly(propylene imine) dendrimer by electrodeposition resulted in an electrochemical sensor which was used to detect lead ions in water to a limit of 1 ppb and a linear response between 2.5 and 40 ppb using square wave anodic stripping voltammetry (SW-ASV). Pb(II) was also removed from spiked water sample using a 40-mm diameter unmodified EG electrode with an applied potential of -1,000 mV for 180 min. A removal efficiency of 99% was calculated from a 150 mL sample. The results obtained in both cases using SW-ASV, correlated with atomic absorption spectroscopy.

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The esterification of stearic acid with p-cresol using modified Indian bentonite clay catalysts has been reported. The reaction was studied over exchanged clays, acid activated clays, exchanged acid activated clays, aluminium pillared clay, aluminium pillared acid activated clay, molecular sieve Al-MCM-41, zeolite H beta, ZrO2, S-ZrO2, p-TSA, montmorillonite K10, and montmorillonite KSF in o-xylene for 6 h. The catalysts were characterized by X-ray diffraction and surface area measurements. The acidity was determined by n-butylamine back-titration method and DRIFTS after pyridine adsorption. Acid activated Indian bentonite (AAIB) was found to be a better catalyst compared to other catalysts in the esterification of stearic acid with p-cresol.

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Glassy carbon electrodes (GCE) and carbon paste electrodes (CPE) were modified with imidazole functionalized polyaniline with the aim to develop a sensor for lead (II) in both acidic and basic aqueous solution. The electrodes were characterized by cyclic voltammetry and differential pulse adsorptive stripping voltammetry. The limit of detections obtained with glassy carbon electrode and carbon paste electrode are 20 ng mL(-1) and 2 ng mL(-1) of lead ion, respectively. An interference study was carried out with Cd(II), As(III), Hg(II) and Co(II) ions. Cd(II) ions interfere significantly (peak overlap) and As(III) has a depressing effect on the lead signal. The influence of pH was investigated indicating that bare and modified GCE and CPE show optimum response at pH 4.0 +/- 0.05.

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The use of titania nanotubes (TiO2-NT) as the working electrode provides a substantial improvement in the electrochemical detection of proteins. A biosensor designed using this strategy provided a robust method to detect protein samples at very low concentrations (C-protein ca 1 ng/mu l). Reproducible measurements on protein samples at this concentration (I-p,I-a of 80 +/- 1.2 mu A) could be achieved using a sample volume of ca 30 mu l. We demonstrate the feasibility of this strategy for the accurate detection of penicillin binding protein, PBP2a, a marker for methicillin resistant Staphylococcus aureus (MRSA). The selectivity and efficiency of this sensor were also validated using other diverse protein preparations such as a recombinant protein tyrosine phosphatase (PTP10D) and bovine serum albumin (BSA). This electrochemical method also presents a substantial improvement in the time taken (few minutes) when compared to conventional enzyme-linked immunosorbent assay (ELISA) protocols. It is envisaged that this sensor could substantially aid in the rapid diagnosis of bacterial infections in resource strapped environments. (C) 2014 Elsevier B.V. All rights reserved.

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In the present study, amino-silane modified layered organosilicates were used to reinforce cyclic olefin copolymer to enhance the thermal, mechanical and moisture impermeable barrier properties. The optimum clay loading (4%) in the nanocomposite increases the thermal stability of the film while further loading decreases film stability. Water absorption behavior at 62 degrees C was carried out and compared with the behavior at room temperature and 48 degrees C. The stiffness of the matrix increases with clay content and the recorded strain to failure for the composite films was lower than the neat film. Dynamic mechanical analysis show higher storage modulus and low loss modulus for 2.5-4 wt% clay loading. Calcium degradation test and device encapsulation also show the evidence of optimum clay loading of 4 wt% for improved low water vapor transmission rates compared to other nanocomposite films. (C) 2014 Elsevier Ltd. All rights reserved.

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This paper presents two approximate analytical expressions for nonlinear electric fields in the principal direction in axially symmetric (3D) and two dimensional (2D) ion trap mass analysers with apertures (holes in case of 3D traps and slits in case of 2D traps) on the electrodes. Considered together (3D and 2D), we present composite approximations for the principal unidirectional nonlinear electric fields in these ion traps. The composite electric field E has the form E = E-noaperture + E-aperture. where E-noaperture is the field within an imagined trap which is identical to the practical trap except that the apertures are missing and E-aperture is the field contribution due to apertures on the two trap electrodes. The field along the principal axis, of the trap can in this way be well approximated for any aperture that is not too large. To derive E-aperture. classical results of electrostatics have been extended to electrodes with finite thickness and different aperture shapes.E-noaperture is a modified truncated multipole expansion for the imagined trap with no aperture. The first several terms in the multipole expansion are in principle exact(though numerically determined using the BEM), while the last term is chosen to match the field at the electrode. This expansion, once Computed, works with any aperture in the practical trap. The composite field approximation for axially symmetric (3D) traps is checked for three geometries: the Paul trap, the cylindrical ion trap (CIT) and an arbitrary other trap. The approximation for 2D traps is verified using two geometries: the linear ion trap (LIT) and the rectilinear ion trap (RIT). In each case, for two aperture sizes (10% and 50% of the trap dimension), highly satisfactory fits are obtained. These composite approximations may be used in more detailed nonlinear ion dynamics Studies than have been hitherto attempted. (C) 2009 Elsevier B.V. All rights reserved.

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An investigation of power frequency (50 Hz) surface partial discharges in dry air, using 21r/3 Rogowski profile electrodes in the low pressure range of 0.067 to 91.333 kPa, shows that for the discharges occurring symmetrically around the electrodes and just outside the uniform field region, the breakdown voltages are 20 to 30% lower than those accounted for by the usual Paschen values. Emphasis, therefore, has been given to modified values of breakdown voltages for any useful calculations. The effect of reduced pressure on inception voltage has been discussed and an attempt has been made to explain the difference between the observed and calculated values on the basis of a pressure-dependent secondary ionization coefficient. It is shown that increasing the insulation thickness in a critical pressure range (0.067 to 0.400 kPa) does not allow any significant increase in the discharge free working stress of the insulation system. At higher pressures (>0.400 kPa) the increase in inception voltage with thickness and pressure follows an equation which is expected to hold for other insulating materials as well.

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The performance of exfoliated graphite (EG)–ruthenium oxide (RuOx) composites as binderless electrodes is evaluated for electrochemical capacitors (ECs). A composite of EG–RuOx is prepared by a modified sol–gel process. The material is characterized using X-ray diffraction and microscopy. Electrochemical capacitors with the composite electrodes in the presence of aqueous sulfuric acid (H2SO4) electrolyte are evaluated using voltammetry, impedance and charge–discharge studies. Cyclic voltammetry reveals very stable current–voltage behaviour up to several thousands of cycles, as well as high specific capacitances, e.g., a few hundreds of farads per gram for the composite that contains 16.5 wt.% RuOx.

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Exfoliated graphite (EG) was modified by covalently attaching dopamine (DA) (3,4-dihydroxyphenethylamine) through amide linkages, using -COOH groups introduced on the EG surface. The modified material was characterized by FT-IR spectroscopy, Xray photoelectron spectroscopy and electrochemical techniques. Composites of DA modified EG dispersed in organically modified silicates were prepared by a sol-get process. Electrodes were fabricated by casting the composites in glass tubes. The sol-gel based electrodes were found to be active for the electrocatalytic oxidation of NADH and biosensing of ethanol in presence of NAD(+) and alcohol dehydrogenase enzyme. The modified composite electrodes were found to be stable for several months. The surface of the electrode could be renewed just by mechanically polishing the electrode using emery sheets. The modified EG was also pressed and restacked in the form of a pellet and the use of this material as a binderless bulk-modified electrode was also demonstrated. The performance of sol-gel derived composite EG electrodes with binderless bulk-modified EG electrodes was compared. (C) 2002 Elsevier Science B.V. All rights reserved.

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Organo-clay was prepared by incorporating different amounts (in terms of CEC, ranging from 134-840 mg of quaternary ammonium cation (QACs) such as hexadecytrimethylammonium bromide (C19H42N]Br) into the montmorillonite clay. Prepared organo-clays are characterized by CHN analyser and XRD to measure the amount of elemental content and interlayer spacing of surfactant modified clay. The batch experiments of sorption of permanganate from aqueous media by organo-clays was studied at different acidic strengths (pH 1-7). The experimental results show that the rate and amount of adsorption of permanganate was higher at lower pH compared to raw montmorillonite. Laboratory fixed bed experiments were conducted to evaluate the breakthrough time and nature of breakthrough curves. The shape of the breakthrough curves shows that the initial cationic surfactant loadings at 1.0 CEC of the clay is enough to enter the permanganate ions in to the interlamellar region of the surfactant modified smectile clays. These fixed bed studies were also applied to quantify the effect of bed-depth and breakthrough time during the uptake of permanganate. Calculation of thermodynamic parameters shows that the sorption of permanganate is spontaneous and follows the first order kinetics.

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Owing to its favourable physical, chemical and rheological properties, densely compacted bentonite or bentonite-sand mix is considered as a suitable buffer material in deep geological repositories to store high level nuclear waste. Iodine-129 is one of the significant nuclides in the high level waste owing to its long half life and poor sorption onto most geologic media. Bentonite by virtue of negatively charged surface has negligible affinity to retain iodide ions. As organo-bentonites are known to retain iodide ions, the present study characterizes hexadecylpyridinium chloride (HDPyCl.H2O) treated bentonite from Barmer India (referred as HDPy+B) for physico-chemical properties, engineering properties and the iodide adsorption behavior of the organo clay. Batch experiments revealed that HDPy+ ions are largely retained (94 % retention) via cation exchange; the ion-exchange process neutralizes the negative surface charge and bridges clay particles leading to reduction in Atterberg limits, clay content and sediment volume. The organo clay retains iodide by Coulombic attraction (at primary sites) and anion exchange (at secondary sites). The free-energy change (Delta G (o) = -25.5 kJ/mol) value indicated that iodide retention by organo clay is favored physical adsorption process. Iodide adsorption capacity of organo clay decreased significantly (85-100 %) on dilution with 50-80 % bentonite. On the other hand, dilution of bentonite with 50 % organo clay caused 58 % reduction in swell potential and 21 % reduction in swell pressure.