Synthesis and characterization of magnetite (Fe3O4)—Polyvinyl alcohol‐based nanocomposites and study of superparamagnetism

The aim of this investigation was to design iron oxide containing nanocomposites which could display superparamagnetic behavior and thus find application in biomedical and allied fields. To achieve the proposed objectives methyl methacrylate was polymerized by a redox system comprising of metabisulphite and persulphate in the immediate presence of a crosslinker, N,N′‐methylene bis acrylamide and a preformed polymer, i.e., polyvinyl alcohol. Into the prepared polymer matrix nanosized magnetite (Fe₃O₄) particles were evenly dispersed by in situ precipitation of Fe²⁺/Fe³⁺ ions. The nanocomposite materials were characterized by techniques like FTIR, SEM, TEM, XRD, and DSC. The magnetic behavior of nanocomposites and bulk magnetite particles was studied under varying applied magnetic fields and their superparamagnetic property was examined. The iron‐oxide polymer nanocomposites were also studied for microhardness. POLYM. COMPOS., 2010. © 2009 Society of Plastics Engineers     

Structural characterizations of diglycerol monomyristate reverse micelles in aromatic solvent ethylbenzene

Using small-angle X-ray scattering (SAXS) we have investigated the shape and size of diglycerol monomyristate (designated as C14G2) nonionic surfactant reverse micelles in aromatic solvent ethylbenzene as a function of surfactant concentration, temperature, and water. When C14G2 is added into ethylbenzene globular type reverse micelles with maximum core diameter ca. 4.5 nm are formed under ambient conditions. The micellar structure (shape and size) did not change with the surfactant concentration. However, an increase in temperature decreased the micellar size due to an increase in the critical packing parameter (cpp). Surfactant becomes more lipophilic upon heating and the micellar curvature tends to become more negative at higher temperature. Addition of a small amount of water caused a significant micellar growth. For instance, incorporation of 0.3% water in the 5% C14G2/ethylbenzene system resulted in the formation of 2.1 time bigger micelles with a small water pool in the micellar core. Besides the micellar shape is modified into an ellipsoidal prolate, whose scenario can be understood in terms of hydration of the surfactant's headgroup. Hydration decreases the cpp and favors micellar growth. An increase of temperature of a water incorporated system decreased the micellar size due to dehydration, which is equivalent to rod-to-sphere type transition.     

Crystallographic evaluation of sodium zirconium phosphate as a host structure for immobilization of cesium

Sodium zirconium phosphate (NZP) is a potential material for immobilization of nuclear effluents. The existence of cesium containing NZP structure was determined on the basis of crystal data of solid solution. It was found that up to ~9.0 wt% of cesium could be loaded into NZP formulations without significant changes of the three-dimensional framework structure. The crystal chemistry of Na_1−x Cs _x Zr₂P₃O₁₂ (x = 0.1–0.4) has been investigated using General Structure Analysis System programming. The CsNZP phases crystallize in the space group R-3c and Z = 6. Powder diffraction data have been subjected to Rietveld refinement to arrive at a satisfactory structural convergence of R-factors. The unit cell volume and polyhedral (ZrO₆ and PO₄) distortion increase with rise in the mole% of Cs⁺ in the NZP matrix. The PO₄ stretching and bending vibrations in the infrared region have been assigned. SEM, TEM, and EDAX analysis provide analytical evidence of cesium in the matrix.     

Deformation and friction of MoS2 particles in liquid suspensions used to lubricate sliding contact

Tribology of a well known solid lubricant molybdenum disulphide is studied here in water and oil medium, over a large range of contact dimensions. Lateral force microscopy is used to identify the deformation modes; intra-crystalline slip, plastic grooving, fragmentation and fracture, of single particles. The medium and agglomeration were found to dictate the deformation mode. Steel on steel tribology lubricated by suspensions of these particles in liquid media was conducted over a range of contact pressure and sliding velocity. A scrutiny of the frictional data with the aid of Raman spectroscopy to identify the transfer film, suggested that the particle size, as it is at contact, is an important tribological parameter. Ultrasonication of the suspension and dispersion of the particle by surfactants were used to control the apriori particle size fed into the suspension. Correspondence of friction data of the gently sonicated suspension with that of the ultrasonicated suspension with dispersants indicated the importance of liquid ingestion by these particles as it controls their mode of deformation and consequent tribology.     

Process optimisation for a ready‐to‐serve breakfast smoothie from a composite milk–sorghum base

A composite milk and sorghum‐based smoothie containing varying levels of sorghum flour (2–4% w/w), sugar (9–11% w/w) and pectin (0.2–0.4% w/w) was optimised by response surface methodology on the basis of sensory (colour and appearance, flavour, consistency, sweetness and overall preference) and physical (viscosity, sedimentation and wheying off) attributes. Flour and pectin levels influenced the flavour, consistency, viscosity and sedimentation significantly. Sugar helped to increase the overall preference and had a positive correlation with sedimentation. An optimised smoothie composition of acceptable quality was obtained with 2.79% (w/w) germinated sorghum flour (GSF), 10.30% (w/w) sugar and 0.35% (w/w) pectin.     

Spectral and laser studies on energy transfer binary dye-doped polymer laser rods

The energy transfer mechanism of two different dyes, C450 as donor and C535 as acceptor incorporated into polymeric matrices, is investigated. The absorption and fluorescence characteristics of C450 and C535 dye-doped polymer modified with ethanol are studied. The results are compared with their respective liquid mixtures. The spectral parameters of C450 and C535 in polymer and the corresponding monomer compositions are obtained. We study the variation of gain for different acceptor concentrations whilst keeping the donor concentration fixed. The gain of acceptor with donor increased and then decreased as the acceptor concentration was increased. Both solid and liquid media showed similar trends. We also study the photobleaching of the dye-doped polymer rod under nitrogen laser excitation.     

Investigation of wide range magnetoresistance in La0.7Ca0.3−xAgxMnO3 (0 ≤ x ≤ 0.2) system

We synthesized magnetoresistive compounds with nominal compositions La_0.7Ca_0.3?xAg_xMnO₃ (0 ≤ x ≤ 0.2) by solid state reaction method with different sintering temperatures. All the samples exhibited orthorhombic structure with variable lattice parameters. The metal-insulator transitions were observed below room temperature in most of the samples. Depending upon the composition and sintering temperature, the samples showed very high magnetoresistance in narrow range or significant magnetoresistance over wide range of temperature. The ac susceptibility measurement revealed compositional dependence of Curie temperature.     

Transdermal and Buccal Delivery of Methylxanthines Through Human Tissue In Vitro

ABSTRACT

We examined the in vitro permeation of central nervous stimulants—caffeine, theophylline, and theobromine across human skin with the aid of six chemical enhancers. It was found that oleic acid was the most potent enhancer for all three methylxanthines. Further optimization studies with different solvents showed that caffeine transport could be enhanced to give flux values up to 585 μg/cm².hr^?1. Theobromine and theophylline delivery rates proved insufficient. An additional study involving a buccal tissue equivalent showed that this membrane was more permeable than skin for all model actives tested and would offer an alternate way of delivery.     

Selective Hydrogenolysis of Glycerol to 1, 2 Propanediol Over Cu–ZnO Catalysts

A series of Cu–ZnO catalysts with varying Cu to Zn weight ratio are prepared by co-precipitation method. The catalysts were characterized by surface area, XRD, TPR and N₂O chemisorption to measure Cu metal area. These catalysts were evaluated for hydrogenolysis of glycerol. The catalyst with Cu to Zn ratio of 50:50 is highly active under relatively low H₂ pressure. The catalysts are highly selective towards 1,2 propanediol (>93%). The glycerol conversion depends upon the bifunctional nature of catalyst where it requires both acidic sites and metal surface. The presence of sufficient amount with small particle size of ZnO and Cu are required for high conversion of glycerol and selectivity to 1,2 propanediol. Different reaction parameters are studied in order to optimize the reaction conditions.     

Novel amorphous precursor densification to transparent Nd:Y2O3 Ceramics

A novel approach of neodymium ion doped yttrium oxide (Nd:Y₂O₃) amorphous precursor compaction and sintering is being reported for the first time. Precursor of 2 at.% Nd³⁺ doped Y₂O₃ was synthesized by gelation of sol of yttrium and neodymium nitrates with l-alanine at 80 °C for 16 h followed by gel combustion in microwave. A part of microwave precursor was heat treated at 700 °C for 5 h to give the partially crystalline Nd:Y₂O₃ amorphous precursor. Thermogravimetric analysis (TGA) of partially crystalline amorphous precursor of Nd:Y₂O₃ gave 8.5% total weight loss indicating removal of maximum organics. X-Ray diffraction (XRD) showed broad peaks indicating incomplete crystallization of cubic Nd:Y₂O₃. Morphology was found to be close to spherical with particles in size range 17–19 nm by TEM. Another part of microwave precursor on calcination at 1000 °C for 3 h led to formation of fully crystalline Nd:Y₂O₃ with particles in size range of 35–85 nm. Both partially crystalline amorphous precursor and fully crystalline Nd:Y₂O₃ were compacted at 400 MPa by cold isostatic press and sintered at 1750 °C for 10 h under vacuum (10^?5 mbar). The partially crystalline Nd:Y₂O₃ amorphous precursor densified to 99% with 65% transmission at 2500 nm (0.5 mm thickness) compared to 96% densification with 34% transmission for fully crystalline Nd:Y₂O₃ without any sintering aids. Retention of cubic phase purity of Y₂O₃ was observed in both the ceramic pellets post sintering by XRD. Good grain fusion with grain growth to ≤2 μm was observed by scanning electron microscope (SEM) for partially crystalline Nd:Y₂O₃ amorphous precursor. Thus partially crystalline Nd:Y₂O₃ amorphous precursor nanopowders, with homogeneous close to spherical fine particles and high reactivity due to ionic mobility of amorphous phase, led to better densification.