Theoretical and experimental studies on the carbon-nanotube surface oxidation by nitric acid: interplay between functionalization and vacancy enlargement

The nitric acid oxidation of multiwalled carbon nanotubes leading to surface carboxylic groups has been investigated both experimentally and theoretically. The experimental results show that such a reaction involves the initial rapid formation of carbonyl groups, which are then transformed into phenol or carboxylic groups. At room temperature, this reaction takes place on the most reactive carbon atoms. At higher temperatures a different mechanism would operate, as evidenced by the difference in activation energies. Experimental data can be partially related to first-principles calculations, showing a multistep functionalization mechanism. The theoretical aspects of the present article have led us to propose the most efficient pathway leading to carboxylic acid functional groups on the surface. Starting from mono-vacancies, it ends up with the synergistic formation of dangling -COOH groups and the enlargement of the vacancies.     

Synthesis,characterization and antimicrobial studies on 13-membered-N6-macrocyclic transition metal complexes containing trimethoprim

Asymmetrical macrocyclic complexes of Mn^II, Co^II, Ni^II, Cu^II and Zn^II have been synthesized by the template process using bis(benzil)ethylenediamine as precursor. Bis(benzil)ethylenediamine reacts with transition metal chlorides and trimethoprim in a 1:1:1 molar ratio in methanol to give several solid metal complexes of the general composition [M(L)X₂] (M = Mn^II, Co^II, Ni^II, Cu^II and Zn^II, L = ligand and X = Cl^?). They were characterized by physicochemical and spectroscopic techniques. Based on analytical, spectral and magnetic moments, all the complexes are identified as distorted octahedral structures. All the complexes are of the [M(L)X₂] type. The shifts of the ν(CN) (azomethine) stretches have been monitored. To find out the donor sites of the ligands, the activity data show that the metal complexes are more potent than the parent ligand. The [M(L)X₂] complexes showed a broad spectrum of antimicrobial activity in vitro against both gram-positive and gram-negative human pathogenic bacterial isolates and the antimicrobial spectrum enhanced only with a combination of metal chlorides and trimethoprim complex. From the results it is imperative that the synthesized macrocyclic [M(L)X₂] complexes exhibit potent broad spectrum antibacterial activity.     

Preparation and characterization of transparent conducting ZnS:Al films

Al-doped ZnS films were deposited using close-spaced evaporation of the powders synthesized by chemical precipitation method. The films were prepared for different Al concentrations in the range 0–10 at.% on glass substrates kept at 300 °C. The effect of Al-doping on ZnS composition, microstructure and optoelectronic properties of as-grown ZnS layers was determined using appropriate techniques. The films were polycrystalline and showed (111) preferred orientation for all the doping concentrations in spite of an additional phase of Al₂S₃ observed at higher dopant levels. The surface morphological studies indicated that the Al incorporation had a considerable effect on the surface roughness of the films. The optical measurements indicated that the optical energy band gap decreased slightly with the increase of dopant concentration without affecting the optical transmittance characteristics significantly. The electrical analysis indicated that the resistivity of the layers changed significantly with the doping concentration in the layers. The change of photoluminescence behaviour of the as-grown ZnS:Al films with dopant concentration was also studied.     

Synthesis and surface chemistry of nano silver particles

In this report, we present a simple wet chemical route to synthesize nano-sized silver particles, and their surface properties are discussed in detail. Silver nano particles of the size 40–80 nm are formed in the process of oxidation of glucose to gluconic acid by amine in the presence of silver nitrate, and the gluconic acid caps the nano silver particle. The presence of gluconic acid on the surface of nano silver particles was confirmed by XPS and FTIR studies. As the nano silver particle is encapsulated by gluconic acid, there was no surface oxidation, as confirmed by XPS studies. The nano silver particles have also been studied for their formation, structure, morphology and size using UV–Visible spectroscopy, XRD and SEM. Further, the antibacterial properties of these nano particles show promising results for E. Coli. The influence of the alkaline medium towards the particle size and yield was also studied by measuring the pH of the reaction for DEA, NaOH and Na₂CO₃.     

Unsteady mixed convection boundary layer flow over a vertical cone with non-uniform slot suction (injection)

The non-similar solution of an unsteady mixed convection laminar boundary layer flow over a vertical cone in the presence of non-uniform surface mass transfer through slot has been obtained while the axis of cone is inline with the flow. The unsteadiness is caused by the time dependent free stream velocity. The governing boundary layer equations are transformed into a non-dimensional form by a group of non-similar transformations. The resulting coupled non-linear partial differential equations have been solved numerically by the combination of quasi-linearization technique and an implicit finite difference scheme. Numerical computations are performed for different values of the parameters to display the velocity and temperature profiles graphically. Both accelerating and decelerating free stream velocities are considered. Numerical results are reported to display the effects of non-uniform single and double slot suction (injection) on skin friction and heat transfer coefficients at the wall. Further, the effects of Prandtl number, buoyancy and mass transfer (suction or injection) parameters at different stream-wise locations for various times on velocity and temperature profiles, and on skin friction and heat transfer coefficients are also presented in this paper.     

Diffusion tensor magnetic resonance imaging of the normal breast

Purpose

The objective of this study was to evaluate diffusion anisotropy of the breast parenchyma and assess the range and repeatability of diffusion tensor imaging (DTI) parameters in normal breast tissue.

Materials and Methods

The study was approved by our institutional review board and included 12 healthy females (median age, 36 years). Diffusion tensor imaging was performed at 1.5 T using a diffusion-weighted echo planar imaging sequence. Diffusion tensor imaging parameters including tensor eigenvalues (λ₁, λ₂, λ₃), fractional anisotropy (FA) and apparent diffusion coefficient (ADC) were measured for anterior, central and posterior breast regions.

Results

Mean normal breast DTI measures were λ₁=2.51×10⁻³ mm²/s, λ₂=1.89×10⁻³ mm²/s, λ₃=1.39×10⁻³ mm²/s, ADC=1.95±0.24×10⁻³ mm²/s and FA=0.29±0.05 for b=600 s/mm². Significant regional differences were observed for both FA and ADC (P<.05), with higher ADC in the central breast and higher FA in the posterior breast. Comparison of DTI values calculated using b=0, 600 s/mm² vs. b=0, 1000 s/mm², showed significant differences in ADC (P<.001), but not FA. Repeatability assessment produced within-subject coefficient of variations of 4.5% for ADC and 11.4% for FA measures.

Conclusion

This study demonstrates anisotropy of water diffusion in normal breast tissue and establishes a normative range of breast FA values. Attention to the influence of breast region and b value on breast DTI measurements may be important for clinical interpretation and standardization of techniques.     

Cyclotriphosphazene Fibre Reinforced Poly(benzoxazine-co-ε-caprolactam) Nanocomposites for Flame Retardant Applications

Cyclophosphazene nanotube(PZT) incorporated poly(benzoxazine-co-ε-caprolactam)(P(BZ-co-CPL)) nanocomposites were developed for improving flame retardant properties. The effects of PZT on the flammability properties of P(BZ-co-CPL) matrix were evaluated through UL-94 flammability test and limiting oxygen index(LOI). The UL-94 results of P(BZ-co-CPL)/PZT hybrid nanocomposites showed V-1 rating, whereas neat P(BZ-co-CPL) showed burning rating. The LOI values are increased from 25.4 to 31.4 for 1.5 wt% PZT incorporated P(BZ-co-CPL) nanocomposite systems. SEM was used to study the char morphology of P(BZ-co-CPL)/PZT after being exposed to UL-94 flammability test. Data from thermal studies indicate that the PZT incorporated P(BZ-co-CPL) systems possess better Tg and thermal degradation behavior when compared to the neat P(BZ-co-CPL). The values of dielectric constant are decreased with increasing temperature. From the values, it is ascertained that the P(BZ-co-CPL)/PZT systems exhibit stable dielectric behavior with regard to variation in temperature. The TEM images ascertain the uniform dispersion of PZT in the P(BZ-co-CPL) matrix.     

Effects of Thermal Radiation on a 3D Sisko Fluid over a Porous Medium Using Cattaneo-Christov Heat Flux Model

This paper investigates the three-dimensional flow of a Sisko fluid over a bidirectional stretching sheet, in a porous medium. By using the effect of Cattaneo-Christov heat flux model, heat transfer analysis is illustrated. Using similarity transformation the governing partial differential equations are transferred into a system of ordinary differential equations that are solved numerically by applying Nachtsheim-Swigert shooting iteration technique along with the 6-th order Runge-Kutta integration scheme. The effect of various physical parameters such as Sisko fluid, ratio parameter,thermal conductivity, porous medium, radiation parameter, Brownian motion, thermophoresis, Prandtl number, and Lewis number are graphically represented.     

ICP-AES analysis of impurities in PuO2 after separation of Pu by TOPO impregnated XAD-4

Nuclear fuels should meet some specified characteristics to achieve their better performance in the reactor. Hence controlling and monitoring of trace level elements in the fuel materials are essential. Atomic emission spectroscopic methods are most popular for the trace level analysis. An ICP-AES procedure is described here for the trace level impurity analysis of PuO₂ produced through PUREX process. To avoid the Pu interference in the impurity analysis, initially the Pu was separated by extraction chromatography using TOPO impregnated XAD-4 resin. Magnitude of Pu interference in the impurities spectra lines was investigated. Moreover the recovery of impurity elements using the resin was established.     

Highly sensitive method for the determination of ropinirole with a lower limit of quantitation of 3.45 pg/mL in human plasma by LC‐ESI‐MS/MS: application to a clinical pharmacokinetic study

A highly sensitive, rapid assay method has been developed and validated for the estimation of ropinirole (RPR) in human plasma with liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in the positive‐ion mode. A solid‐phase process was used to extract RPR and citalopram (internal standard, IS) from human plasma. Chromatographic separation was operated with 0.2% ammonia solution:acetonitrile (20:80, v/v) at a flow rate of 0.50 mL/min on a Hypurity C₁₈ column with a total run time of 3.2 min. The MS/MS ion transitions monitored were 261.2 → 114.2 for RPR and 325.1 → 209.0 for IS. Method validation and clinical sample analysis were performed as per FDA guidelines and the results met the acceptance criteria. The lower limit of quantitation achieved was 3.45 pg/mL and the linearity was observed from 3.45 to 1200 pg/mL. The intra‐day and inter‐day precisions were in the range of 4.71–7.98 and 6.56–8.31%, respectively. This novel method has been applied to a pharmacokinetic study of RPR in humans. Copyright © 2008 John Wiley & Sons, Ltd.