Tetrakis(1‐naphthylamino)silane and its tetrahydrofuran trisolvate

In both title structures, C₄₀H₃₂N₄Si and C₄₀H₃₂N₄Si·3C₄H₈O, the angles around the Si atom deviate significantly from the tetrahedral value [104.34 (7)–116.63 (7)° in the nonsolvate and 99.91 (15)–116.85 (15)° in the solvate]. The amino H atoms in the solvated structure are involved in hydrogen bonding with two of the tetrahydrofuran solvent molecules.     

Alkylation of catechol with methanol to guaiacol over sulphate-modified zirconia solid acid catalysts

A series of sulphate-promoted ZrO₂ solid acid catalysts with different contents of SO₄ ²⁻ were calcined at 450°C in air for 4 h and tested for the liquid-phase alkylation of catechol to guaiacol in a fixed-bed down-flow reactor. The 5 wt.% SO₄ ²⁻ on ZrO₂ showed the best conversion (82%) and selectivity for guaiacol (84%) at 200°C and 1 bar pressure. A smooth correlation was observed between the catalytical activity and surface acidity of sulphated zirconia. Based on our results, a surface mechanism is proposed.     

Comparison of compositional and morphological atom-probe tomography analyses for a multicomponent Fe-Cu steel.

A multicomponent Fe-Cu based steel is studied using atom-probe tomography. The precipitates are identified using two different methodologies and subsequent morphological and compositional results are compared. The precipitates are first identified using a maximum separation distance algorithm, the envelope method, and then by a concentration threshold method, an isoconcentration surface. We discuss in detail the proper selection of the parameters needed to delineate precipitates utilizing both methods. The results of the two methods exhibit a difference of 44 identified precipitates, which can be attributed to differences in the basis of both methods and the sensitivity of our results to user-prescribed parameters. The morphology of the precipitates, characterized by four different precipitate radii and precipitate size distribution functions (PSDs), are compared and evaluated. A variation of less than approximately 8% is found between the different radii. Two types of concentration profiles are compared, giving qualitatively similar results. Both profiles show Cu-rich precipitates containing Fe with elevated concentrations of Ni, Al, and Mn near the heterophase interfaces. There are, however, quantitative disagreements due to differences in the basic foundations of the two analysis methods.     

Photoactive Titania Float for Disinfection of Water; Evaluation of Cell Damage by Bioanalytical Techniques

A photoactive float was fabricated with the modified titania to cause a feasible disinfection of water, contaminated with E. coli. The commercially available titania was doped with neodymium by pulverization technique to enhance its activity in sunlight and a multiapproach technique was used to evaluate the extended efficiency of the doped sample. X‐ray diffraction patterns depicted the retention of anatase phase on doping and the existence of neodymium was confirmed by the energy dispersive atomic X‐ray analysis and the X‐ray photoelectron spectroscopy. Transmission electron microscopy and Bruner–Emmett–Teller analysis depicted a marginal increase in the particle size and a decrease in the surface area, respectively. Doping induces semiconductor behavior with lower band energy that could respond to visible light and exhibit better disinfection activity. The “f” and “d” transitions of the lanthanide in doped sample caused new electronic behavior of trapping/detrapping effect together with bandgap narrowing. The amount of malondialdehyde, protein, DNA and RNA released on destruction of E. coli was observed to be 0.915 × 10^?3 μg mL^?1, 859.912 μg mL^?1, 20.173 μg mL^?1 and 1146.073 μg mL^?1, respectively. The above analytical methods along with standard plate count method substantiated the enhanced disinfection efficiency of the doped sample in sunlight.     

Siloxane polymers containing azo moieties synthesized by click chemistry for photo responsive and liquid crystalline applications

Three new types of siloxane‐based photoactive liquid crystalline polymers containing azo side groups were synthesized through the click chemistry route. The polymers having molecular weight range of 14,000–34,000 g mol^?1 were soluble in most of the polar solvents like chloroform, tetrahydrofuran, dimethylformamide, dimethyl sulfoxide, and dichloromethane. The photoresponsive trans–cis photoisomerization under UV radiation and cis–trans relaxation process in dark for the polymers were studied. The isomerization rate constants were found to be 0.01–0.04 sec^?1 and 1.16*10^?4–4.67*10^?4 sec^?1, respectively. It has been noted that the polymers showed high intensity absorption for n‐π* in chloroform. Both trans and cis forms of azide monomers having azo moiety exhibited molar extinction coefficient ( ? _max) in the range of 22,000–33,000 L mol^?1 cm^?1. The thermotropic behavior of the polymers was studied by polarizing optical microscope (POM) and differential scanning calorimetry (DSC) experiments. Polymer P1 showed liquid crystalline textures of nematic droplets, whereas P2 showed smectic focal conic texture and nematic droplets. Polymer P1 was also studied for photomechanical bending on exposure to UV radiation. The polymers showed initial degradation temperature in the range of 210–275°C. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012     

Click chemistry‐based synthesis of azo polymers for second‐order nonlinear optics

Four linear polymers containing pendant azo moiety were synthesized through click chemistry for second‐order nonlinear optical study. The polymers were found soluble in most of the polar organic solvents such as tetrahydrofuran (THF), chloroform, and dimethyl formamide (DMF). The polymers showed thermal stability up to 300 °C and glass transition temperatures (T_g) in the range of 120–140 °C. The molecular weights (M_w) of these polymers (measured by gel permeation chromatography) were in the range 37,900–55,000 g/mol. The polymers were found to form optically transparent films by solution casting from THF solution. Order parameters were calculated from UV–vis absorption spectra. The morphology changes in the films after poling were characterized by atomic force microscopy. The angular dependence, temperature dependence, and time dependence of second harmonic generation (SHG) intensity were obtained by using 1064 nm Nd:YAG laser. The SHG intensity remained unchanged up to 95 °C. At room temperature, it remained stable up to 8 days after initial drop of about 14%. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012     

Magnetic nanoparticle‐tethered Schiff base–palladium(II): Highly active and reusable heterogeneous catalyst for Suzuki–Miyaura cross‐coupling and reduction of nitroarenes in aqueous medium at room temperature

As a continuation of our efforts to develop new heterogeneous nanomagnetic catalysts for greener reactions, we identified a Schiff base–palladium(II) complex anchored on magnetic nanoparticles (SB‐Pd@MNPs) as a highly active nanomagnetic catalyst for Suzuki–Miyaura cross‐coupling reactions between phenylboronic acid and aryl halides and for the reduction of nitroarenes using sodium borohydride in an aqueous medium at room temperature. The SB‐Pd@MNPs nanomagnetic catalyst shows notable advantages such as simplicity of operation, excellent yields, short reaction times, heterogeneous nature, easy magnetic work up and recyclability. Characterization of the synthesized SB‐Pd@MNPs nanomagnetic catalyst was performed with various physicochemical methods such as attenuated total reflectance infrared spectroscopy, UV–visible spectroscopy, inductively coupled plasma atomic emission spectroscopy, energy‐dispersive X‐ray spectroscopy, field‐emission scanning electron microscopy, transmission electron microscopy, powder X‐ray powder diffraction, thermogravimetric analysis and Brunauer–Emmett–Teller surface area analysis.