Sulfite determination using sulfite oxidase biosensor based glassy carbon electrode coated with thin mercury film

The preparation of sulfite biosensor by immobilization of sulfite oxidase on a glassy carbon electrode coated with mercury thin film is described. Dissolved oxygen can be readily reduced at the glassy carbon electrode coated with mercury thin film. The working principle of the biosensor was based on monitoring decrease in the peak current due to the depletion in dissolved oxygen concentration according to the reaction of sulfite oxidase.     

Dispersion polymerization of methyl methacrylate in supercritical carbon dioxide using a silicone‐containing fluoroacrylate stabilizer

Free radical dispersion polymerization of methyl methacrylate (MMA) was carried out in supercritical carbon dioxide (scCO₂) using poly{(heptadecafluorodecyl acrylate)‐co‐3‐[tris(trimethylsilyloxy)silyl]propyl methacrylate} (p(HDFDA‐co‐SiMA)) as stabilizer. Dry, fine powdered spherical poly(methyl methacrylate) (pMMA) particles with well‐defined sizes were produced. The resulting high yield of spherical and relatively uniform micron‐size pMMA particles was formed utilizing various amounts of p(HDFDA‐co‐SiMA) random copolymer. The particle diameter was shown to be dependent on the weight percent of the stabilizer added to the system. The effects of varying the concentration of stabilizer (1–7 wt%), reaction time (4–12 h) and pressure (15–35 MPa) upon the polymerization yield, molar mass and morphology of pMMA were investigated. Copyright © 2005 Society of Chemical Industry     

Hydrothermal Synthesis of Polyoxometalate Containing Cobalt Ion,and Its Polyurethane Composites for Dielectric Material Applications

ABSTRACT

Polyurethane (PU) composites were prepared with different diisocyanate and diol compounds by adding cobalt ion-based polyoxometalate (Co-POM) as reinforcement. For the determination of using potential in microelectronic applications, the dielectric behavior and dielectric constant of these PU composites were investigated and compared to pure polyurethane structures. For this aim, firstly, Co-POM with Keggin structure was obtained from ammonium heptamolybdate, 1,10-phenanthroline ligand and a cobalt (II) salt by hydrothermal synthesis technique. Then, polyurethane/Co-POM composites (PU/Co-POM) were prepared with ethylene glycol, nonaromatic diisocyanate and different amounts of Co-POM reinforcement (1%, 3%, 5% and 10%, w/w) by in situ polymerization and mix-blend technique. Obtained PU/Co-POM composites were characterized in detail by infrared spectroscopy, Elemental Mapping, Energy-dispersive X-ray spectroscopy (EDX) and X-ray powder diffraction (XRD) spectroscopy. The surface structure, morphology and roughness of PU/Co-POM composites were investigated by SEM and AFM analysis. The elemental maps of the PU/Co-POM surface were examined by EDX elemental mapping analysis methods. Thermal stability, Tg values and thermal decomposition temperatures of PU/Co-POM structures were determined by different thermal analysis techniques. Thermal analysis results showed that the PU/Co-POM composites are thermally stable up to approximately 200°C and Tg values of synthesized PU composites are seen between 54.72°C and 75.15°C. The dielectric properties and dielectric constants of the PU/Co-POM composites were determined in the frequency range 1 Hz to 1000 kHz at room temperature using impedance analyzer. Dielectric constants of these composites were ranged from 5.50 to 9.26 according to their polarizability and H-bonding ability of PU matrix structure. According to the dielectric measurements, the dielectric constants of the PU/Co-POM structures were significantly decreased compared to the pure PU structures.     

Determination of fluorine in milk samples via calcium-monofluoride by electrothermal molecular absorption spectrometry

The determination of fluorine in milk samples via the molecular absorption of calcium mono-fluoride (CaF) was performed using a HR-CS-ETAAS. For this purpose, calcium was pipetted to graphite furnace together with samples. The amount of Ca and the graphite furnace program were optimised. Fluorine was determined in pyrolytically coated platforms at 606.440 nm applying a pyrolysis temperature of 700 °C and a molecule forming temperature of 2250 °C. Finally, applying standard addition technique, F contents of several milk samples were determined. The results obtained by linear calibration and standard addition techniques were significantly different which can be attributed to non-spectral interferences in milk due to matrix concomitants. Therefore, in order to tolerate the errors, the F contents of several milk samples were determined applying standard addition technique. However, since the ingredients of milk samples change for different kinds, the F in each sample was determined from its own standard addition curve. The range of F content for the milk samples were 0.027–0.543 μg mL⁻¹. The limit of detection and characteristic mass of the method were 0.26 and 0.13 ng of F, respectively.     

Superparamagnetic iron oxide nanoparticle attachment on array of micro test tubes and microbeakers formed on p-type silicon substrate for biosensor applications

A uniformly distributed array of micro test tubes and microbeakers is formed on a p-type silicon substrate with tunable cross-section and distance of separation by anodic etching of the silicon wafer in N, N-dimethylformamide and hydrofluoric acid, which essentially leads to the formation of macroporous silicon templates. A reasonable control over the dimensions of the structures could be achieved by tailoring the formation parameters, primarily the wafer resistivity. For a micro test tube, the cross-section (i.e., the pore size) as well as the distance of separation between two adjacent test tubes (i.e., inter-pore distance) is typically approximately 1 μm, whereas, for a microbeaker the pore size exceeds 1.5 μm and the inter-pore distance could be less than 100 nm. We successfully synthesized superparamagnetic iron oxide nanoparticles (SPIONs), with average particle size approximately 20 nm and attached them on the porous silicon chip surface as well as on the pore walls. Such SPION-coated arrays of micro test tubes and microbeakers are potential candidates for biosensors because of the biocompatibility of both silicon and SPIONs. As acquisition of data via microarray is an essential attribute of high throughput bio-sensing, the proposed nanostructured array may be a promising step in this direction.     

Characterization of BPN Pyrotechnic Composition Containing Micro‐ and Nanometer‐Sized Boron Particles

The effect of micro‐ and nanometer‐sized boron particles on boron‐potassium nitrate (BPN) ignition composition was investigated in this paper. As a starting point, thermochemical calculations were made to determine the most promising ignition compositions. Both stoichiometric and fuel‐rich formulations of BPN were produced to observe the performance variation due to boron content. Particle morphology of boron particles and the surface structure of the ignition compositions were investigated by SEM. The influence of micro‐ and nanometer‐sized boron particles on the calorific value, sensitivity properties, and pressure buildup of compositions were investigated. Sensitivity tests showed that all compositions were safe enough for handling. It was seen that although nanometer‐sized boron particles enhanced calorific value and pressurization rate, they did not have a contribution on the maximum pressure level. The maximum adiabatic flame temperature was attained by the stoichiometric composition, but in practice, the stoichiometric composition resulted in much lower performance than the fuel rich composition. Possible reasons for these behaviors of the compositions were discussed in the paper.     

Synthesis and Dielectric Properties of Polyimide-Titania Hybrid Composites

A new class of polyimide-titania (TiO₂) composites with chemical bonds between the polyimide and titania system has been synthesized by the sol–gel reaction and characterized. The hybrid composite films were obtained by the reaction of lysine-organotitane monomer, which is formulated as [(EtO)₃Ti (lysinate)]_2, followed by polycondensation with dianhyride in N-methyl-2-pyrrolidone (NMP) solution, followed by heating at 100, 200, and 300 °C. The presence of chemical bonds between polyimide (PI) and titania has great effect on the properties of polyimide films, especially on their thermal and dielectric properties. The dielectric constants of the resultant nanocomposites are lower than the usual polyimide films due to the increased free volume and less polar Ti–O–Ti groups, and can be tuned by varying the molar ratio of tetraethoxysilane (TEOT) in the feed. The polyimide units offer additional advantages of imparting thermal and mechanical strength.     

Reuse of leachate waste-water using MEMBIOR technology and reverse osmosis

This article shows that it is technically possible to produce high-grade quality water, which can be used for process water (as a substitute for ground-water), from a leachate waste-water stream. By using external MEMBIOR technology on the leachate waste-water, high removal efficiencies are obtained for both organic compounds and for nitrogen. High membrane fluxes are also obtained, which were stable during the last two months of a test period.     

Thermogravimetric and resistivity study of Ex situ and In situ poly(methyl methacrylate)/carboxylic acid group functionalized multiwall carbon nanotubes composites

Polymer composites based on poly(methyl methacrylate) (PMMA)/carboxylic acid group functionalized multiwall carbon nanotubes (MWCNT) were prepared by the ex situ and in situ techniques with 0.05% loading by weight. Composite films were fabricated by solvent casting method. Electrical conductivity of the composites as well as of the neat PMMA polymer was measured in the temperature range 333 K to 423 K. Neat PMMA samples prepared by the same method showed complete insulating behavior. Ex situ technique leads to a lower value of percolation threshold. Infrared spectroscopy was used to analyze the effect of functionalization of MWCNT on the interfacial bonding of PMMA and MWCNT. Thermogravimetric analysis revealed that the maximum degradation temperature has been shifted to higher region for in situ composites compared to PMMA itself—and the ex situ composites indicated better thermal stability. X‐ray diffraction study of composites also indicates that in situ composites functionalization incorporated MWCNT particles in the polymer chain. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011