Mesoporous TiO2 core-shell spheres composed of nanocrystals with exposed high-energy facets: facile synthesis and formation mechanism

A facile new method that combines electrospray and hydrothermal treatment is used to prepare mesoporous core-shell TiO(2) spheres with high specific surface areas and high pore volumes. Interestingly, the resulting TiO(2) spheres are composed of anatase TiO(2) nanocrystals with exposed step-like {001} and smooth {010} facets. The percentage of exposed {001} facets can be adjusted by changing the experimental parameters used in the electrospray and hydrothermal treatment processes, such as the contents of poly(N-vinyl-2-pyrrolidone) and acetic acid. The combination of high specific surface area (>100 m(2) g(-1)), high pore volume (>0.30 cm(3) g(-1)), useful pore size (10-15 nm), spherical core-shell structure, and exposed high energy facets makes these TiO(2) spheres an important candidate for use in many photoelectrochemical applications. The formation mechanism of the mesoporous TiO(2) spheres is also studied. The great advantage of this method is that interesting and complicated mesoporous superstructures can be prepared using electrospray technology.     

Simultaneous two- and three-component determinations in multicomponent mixtures by extraction-spectrophotometry and thermochromism of ion-association complexes

A selective method of determination of amines and quaternary ammonium salts by solvent extraction and thermochromism of ion-association complexes has been established. The method is based on the formation of ion-association species with tetrabromophenolphthalein ethyl ester and the thermochromism effect in the organic phase at low temperature. The absorbance of the red amine charge-transfer complexes decreases quantitatively (DeltaA) with increase in temperature (DeltaT), and Delta A Delta T is characteristic of a particular species. This characteristic has been applied for the sensitive and selective determination of amines. The absorbance of the blue quaternary ammonium ion-association complexes does not vary with temperature, however, and the quaternary ammonium compounds can be determined without interference by amines because of the disappearance of the red species at 60 degrees . Methylephedrine, diphenhydramine, ephedrine (amines), benzethonium and/or berberine (quaternary ammonium compounds) in two- and three-component mixtures can be determined by using the thermochromism effect. The method is highly selective, sensitive and reproducible.     

Determination of molecular weight distribution of nylon 12 by gel permeation chromatography

Molecular weight distribution of Nylon 12 was determined with hexafluoroisopropanol/toluene mixture as eluent by gel permeation chromatography. Calibration curve for Nylon 12 was easily obtained from that of polystyrene because the method of universal calibration was applicable among these polymers. The molecular weight distributions of Nylon 12 were always broader than expected by the theory of polymerization, i.e., most probable distribution. This result was not caused by broadening effect in gel permeation chromatography, but by polymerization itself.     

Stereoselective adduct formation of α-acylcamphorato-copper(II) chelates with some chiral Lewis bases

The formation constants of the mono-adducts of α-acylcamphorato-copper(II) chelates such as (+)-Cu(facam)₂, (?)-Cu(facam)₂, (+)-Cu(hfbc)₂ and (?)-Cu(hfbc)₂ with some chiral Lewis bases were determined spectrophotometrically in benzene. In order to compare the adduct formation constants obtained with the (+)- and (?)-forms, some pairs of chiral Lewis bases such as 1-amino-2-propanol [(R)(?), (S)(+)], 1-(α-naphthyl)ethylamine [(R)(+), (S)(?)], α-phenyl ethylamine [(R)(+), (S)(?)] and also quinine and quinidine were examined as neutral ligands. Although not very pronounced, the effects of combinations obtained for (+)- or (?)-Cu(II) chelates and (+)- or (?)-ligands indicate that formation constants obtained by the formation of adducts with the ligands having different directions of the optical rotation seems to be superior to those with the same direction.     

Reactions of group IV organometallic compounds : XXVII. Some reactions of [(trimethylsilyl)imino]phosphorane

The reaction of [(trimethylsilyl)imino]methyldiphenylphosphorane: Ph₂MePNSiMe₃ (I) with several acid anhydrides or alkyl isocyanates took place by the simple cleavage of silicon-nitrogen bond. In contrast the interaction of (I) with phenyl isocyanate, isothiocyanate or carbon disulphide led to addition-elimination reactions of the Wittig type. Detailed investigation in the case of phenyl isocyanate indicated the usual elimination of Ph₂MePO is suppressed by the strong affinity of the trimethylsilyl group for anionic oxygen atom.     

Absorption and excretion of suprofen in both sexes of rats, guinea pigs, and rabbits

DL-2-(4-2-Thienylcarbonyl)phenyl)propionic acid (suprofen) was rapidly absorbed in both sexes of rats, guinea pigs, and rabbits after oral administration. Blood levels after a single dose of 2 mg/kg 3H-suprofen in all the animals reached maxima within 15 min, and elimination of the 3H from blood was rapid; the radioactivity was mostly excreted in the urine and feces within 24 h after dosing.     

Synthesis of poly(2,5-dimethylphenylene sulfide) through oxidative polymerization of sulfur chloride with p-xylene

Poly(2,5-dimethylphenylene sulfide) was prepared by oxidative polymerization of sulfur chloride with p-xylene using 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) as an oxidizing agent. The reaction proceeded efficiently under atmospheric pressure and at room temperature. The polymer formed had a high melting temperature and linear structure which was confirmed by spectroscopies. The effects of reaction time, solvent, temperature and oxidizing agent on polymerization are also discussed.     

Photo-switchable ion and enzyme sensors. Photoinduced potentiometric response of glassy carbon electrode coated with polymer or polymer/enzyme dual membrane

Photo-switchable ion and enzyme sensors were fabricated by the use of glassy carbon electrode coated with nonactindoped or enzyme modified poly(vinyl chloride) (PVC) membranes. The ion sensor with nonactin-doped PVC membrane, which contained spirobenzopyran as the photosensitive dye, exhibited a potentiometric photoresponse to NH4+ ion in the solution. The dynamic range of the NH4+ ion sensor was 10(-7)--10(-3) M. Urea, adenosine, and asparagine sensors were prepared by coating the surface of the NH4+-ion sensor with urease, adenosine deaminase, and asparaginase membranes, respectively. These enzyme sensors could be used for determining the substrates at the micro mole level. The performance characteristics of these sensors were compared with those previously prepared membrane electrode sensors.     

Molecular interactions between lipid bilayers and a water-soluble polymer

Molecular interactions between lipid bilayers (liposomes) and chondroitin sulfate C (CS), a water soluble polymer, have been investigated in terms of zeta-potential, particle size, microscopic-viscosity, microscopic-polarity of liposomes and permeability of calcein. Microscopic morphology is dramatically changed by the addition of CS to the positively charged liposomes (Pos.L), while it is not changed by the addition to uncharged liposomes (Unc.L) or negatively charged liposomes (Neg.L). The absolute value of the particle size of Pos.L increases with the addition of CS, while the zeta- potential of Pos.L decreases. Permeability of Pos.L decreases with an increase in the concentration of CS. Phase transition temperature of Pos.L is changed after the addition of CS. These values, however, are not changed for the other liposomes by the addition of CS. The results of gel filtration chromatography show that CS is absorbed on the Pos.L surface. Microscopic viscosity is also increased by the addition of CS to Pos.L due to the adsorption of CS.