Hg(II) immobilized MWCNT graphite electrode for the anodic stripping voltammetric determination of lead and cadmium

The preparation of Hg(II)-modified multi walled carbon nanotube (MWCNT) by reaction of oxidized MWCNT with aqueous HgCl₂ was carried out. The Hg(II)-modified multi walled carbon nanotube (Hg(II)/MWCNT) dispersed in Nafion solution was used to coat the polished graphite electrode surface. The Hg(II)/MWCNT modified graphite electrode was held at a cathodic potential (−1.0 V) to reduce the coordinated Hg(II) to Hg forming nanodroplets of Hg. The modified electrode was characterized by FESEM/EDAX which provided useful insights on the morphology of the electrode. The SEM images showed droplets of Hg in the size of around 260 nm uniformly distributed on the MWCNT. Differential pulse anodic stripping voltammetry (DPASV) and electrochemical impedance spectroscopy were used to study the Hg(II) binding with MWCNT. Differential pulse anodic stripping voltammetry of ppb levels of cadmium and lead using the modified electrode yielded well-defined peaks with low background current under a short deposition time. Detection limit of 0.94 and 1.8 ng L⁻¹ were obtained following a 3 min deposition for Pb(II) and Cd(II), respectively. Various experimental parameters were characterized and optimized. High reproducibility was observed from the RSD values for 20 repetitive measurements of Pb(II) and Cd(II) (1.7 and 1.9%, respectively). The determination of Pb(II) and Cd(II) in tap water and Pb(II) in human hair samples was carried out. The above method of fabrication of Hg(II)/MWCNT modified graphite electrode clearly suggests a safe route for preparing Hg immobilized electrode for stripping analysis.     

High-speed, high-resolution Fourier-domain optical coherence tomography system for retinal imaging in the 1060 nm wavelength region

A high-speed (47,000 A-scans/s), ultrahigh axial resolution Fourier domain optical coherence tomography (OCT) system for retinal imaging at approximately 1060 nm, based on a 1024 pixel linear array, 47 kHz readout rate InGaAs camera is presented. When interfaced with a custom superluminescent diode (lambda(c) = 1020 nm, Deltalambda = 108 nm, Pout = 9 mW), the system provides 3.3 microm axial OCT resolution at the surface of biological tissue, approximately 4.5 microm in vivo in rat retina, approximately 5.7 microm in vivo in human retina, and 110 dB sensitivity for 870 microW incident power and 21 mus integration time. Retinal tomograms acquired in vivo from a human volunteer and a rat animal model show clear visualization of all intraretinal layer and increased penetration into the choroid.     

Catalytic Oxidation of Dopamine at a Nickel Hexacyanoferrate Surface Modified Graphite Wax Composite Electrode Coated with Nafion

A chemically modified electrode was successfully fabricated by means of depositing a thin layer of nickel hexacyanoferrate (NiHCF) on an amine adsorbed graphite paraffin wax composite electrode using a new approach. The electrode was further coated with Nafion. The electrochemical characteristics of the modified electrode were studied using cyclic voltammetry and electrochemical impedance spectroscopy (EIS). The modified electrode catalyzed dopamine (DA) oxidation in the concentration range of 1.5×10^?6 to 1.2×10^?3 M without the interference from ascorbic acid (AA). A detection limit of 4.9×10^?7 M was obtained for DA in the presence of AA with a correlation coefficient of 0.9972 based on S/N=3. Flow injection analysis was used for the determination of dopamine with excellent reproducible results. The analytical utility of the sensor was evaluated for detection of DA in urine.     

Impedance and Electric Modulus Analysis of Cd0.6Zn0.4Te Thin Films

Cd_0.6Zn_0.4Te thin films were deposited by single source vacuum evaporation technique. The impedance of polycrystalline Cd_0.6Zn_0.4Te thin films has been measured as a function of frequency. The experimental data were measured in the temperature range of 300 – 445K and have been analyzed in the complex plane formalism and suitable equivalent circuits have been proposed in different regions. The values of resistance and capacitance of bulk and grain boundary contributions have also independently calculated from the peak of spectroscopic plots. The role of bulk and grain boundary in the overall conduction process has been discussed with realistic justification. The frequency analysis of ac conduction properties showed distribution of relaxation times due to the presence of multiple grain boundaries in the films. The activation energy calculated from the complex impedance analyses was found to be 0.29eV. The values of activation energies decrease with increase in frequency and are in agreement with that calculated from the impedance plot.     

Synthesis and Characterization of Process Related Impurities of (±)‐Milnacipran

Milnacipran is a cyclopropane derivative, used as an anti depressant drug. During the process development of milnacipran, four process related potential impurities were detected in high performance liquid chromatography. All these impurities were identified, synthesized and subsequently characterized by their respective spectral data (IR, LC‐MS, ¹H NMR, and ¹³C NMR) as described in this article.     

Multifractal scaling of crack images from pyroligneous acid dried sludge

Tannery effluent (sludge, wastewater) is treated by natural way. The waste sludge has been taken for two treatment process. The alkali chemicals are neutralized by pyroligneous acid which is obtained by pyrolysis process of wood. This sludge is sent out for drying. The dried sludge contains some crack pattern formation. Photographs were used to record two sludge cracking surfaces. Experiment has been performed to study the fracture pattern formation in thin film sludge. We studied changes of crack surface of a sludge by image analysis and also assessed applicability of fractal scaling to crack surfaces. The calculated crack surface dimension shows that the fracture surface exhibit fractal structure. Image size was 256 × 256 pixels. MFA (multifractal analysis) was carried out to the method of moments, i.e., the probability distribution was estimated for moments ranging from ?150 < q < 150 and the generalized dimension were calculated from the log/log slope of the probability distribution for the respective moments over box sizes. Generalized dimension D(q) were attained for this box size range, which are capable of characterizing heterogeneous spatial crack structure. Multifractal spectra analyzed two fracture surface of the image and results were indicated that the width of spectra increases due to pyroligneous acid. Multifractal method is sensitive enough to measure the fracture distribution and can be seen as a different approach for changing research of crack images of manure sludge drying.     

UV,violet and blue‐green luminescence from RF sputter deposited ZnO:Al thin films

The mechanism of ultraviolet (UV), violet and blue green emission from ZnO:Al (AZO) thin films deposited at different radio frequency (r.f.) powers on glass substrates was investigated. The structure and surface morphology of AZO films have also been observed. The optical transmittance spectra shows more than 80% transmittance in the visible region and the band gap is found to be directly allowed. From the photoluminescence measurement, intense UV and blue green luminescence is obtained for the samples deposited at higher sputtering powers. The mechanism of luminescence suggests that UV luminescence of AZO thin film is related to the transition from near band edge to the valence band and the concentration of antisite oxide (O_zn) increases with increase in r.f. power which in turn increases the intensity of green band emission while the violet PL is due to the defect level transition in the grain boundaries of AZO films. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Hot-injection synthesis of iron/iron oxide core/shell nanoparticles for T2 contrast enhancement in magnetic resonance imaging

Here we report a new, bench-top synthesis for iron/iron oxide core/shell nanoparticles via the thermal decomposition of Fe(η(5)-C(6)H(3)Me(4))(2). The iron/iron oxide core/shell nanoparticles are superparamagnetic at room temperature and show improved negative contrast in T(2)-weighted MR imaging compared to pure iron oxides nanoparticles, and have a transverse relaxivity (r(2)) of 332 mM(-1) s(-1).     

Amperometric determination of paracetomol by a surface modified cobalt hexacyanoferrate graphite wax composite electrode

A stable electro active thin film of cobalt hexacyanoferrate (CoHCF) was deposited on the surface of an amine adsorbed graphite wax composite electrode using a simple method. Cyclic voltammetric experiments showed two pairs of well defined peaks for this CoHCF modified electrode which exhibited excellent electrocatalytic property for the oxidation of paracetomol at a reduced overpotential of 100 mV and over a concentration range of 3.33 × 10⁻⁶ to 1.0 × 10⁻³ M with a slope of 0.208 μA/μM with good sensitivity. The influence of the supporting electrolyte on peak current and peak potential were also obtained in addition with effects of common interference (e.g., ascorbic acid) on the response of the modified electrode. Various parameters that influence the electrochemical behavior of the modified electrode were optimized by varying scan rates and pH. Electrochemical impedance spectroscopy studies suggested that the electrode reaction of the CoHCF film is mainly controlled by transport of counter ion. The immobilized CoHCF maintained its redox activity showing a surface controlled electrode reaction with the electron transfer rate constant (K_s) of 0.94 s⁻¹ and charge transfer coefficient of 0.42. Hydrodynamic and chronoamperometric studies were done to explore the utility of the modified electrode in dynamic systems. The results of the differential pulse voltammetry (DPV) using the modified electrode was applied for the determination of paracetomol in commercially available tablets. The results obtained reveal that the electrode under study could be used as an effective sensor for online monitoring of paracetomol.     

Free vibration of layered cylindrical shells filled with fluid

The vibration of the layered cylindrical shells filled with a quiescent, incompressible, and inviscid fluid is analyzed. The governing equations of the cylindrical shells are derived by Love’s approximation. The solutions of the displacement functions are assumed in a separable form to obtain a system of coupled differential equations in terms of the displacement functions. The displacement functions are approximated by Bickley-type splines. A generalized eigenvalue problem is obtained and solved numerically for the frequency parameter and an associated eigenvector of the spline coefficients. Two layered shells with three different types of materials under clamped-clamped (C-C) and simply supported (S-S) boundary conditions are considered. The variations of the frequency parameter with respect to the relative layer thickness, the length-to-radius ratio, the length-to-thickness ratio, and the circumferential node number are analyzed.