Grafting of organosilane derived from 3-glycidoxypropyltrimethoxysilane and thiourea onto magnesium phyllosilicate by sol–gel process and investigation of metal adsorption properties

A layered inorganic–organic magnesium silicate (Mg-GTPS-TU) has been successfully synthesized by using sol–gel based precursor under mild temperature conditions and a new silylaing agent (GTPS-TU) derived from 3-glycidoxypropyltrimethoxysilane (GTPS) and thiourea (TU) as the silicon source. The hybrid material was characterized through elemental analysis, infrared spectroscopy, X-ray diffractometry, thermogravimetry, and carbon and silicon solid-state nuclear magnetic resonance spectroscopy. The result confirmed the attachment of organic functionality to the inorganic silicon network. The inter-lamellar distance for the hybrid material was found to be 18.8 Å. Metal adsorption characteristics follows Cr(III) >Mn(II)>Zn(II) with more affinity towards Cr(III) in dilute aqueous solution. Evaluation of thermodynamic parameters ΔH and ΔS for Cr(III) were found to be 25.44 J mol⁻¹ and 79.9 J mol⁻¹ K⁻¹, respectively, indicating adsorption process to be endothermic in nature. The negative value of ΔG indicated the feasibility and spontaneity of ongoing adsorption process at relatively higher temperature. The presence of multiple coordination sites in the attached organic functionality expresses the potentiality of the hybrid material containing new silylating agent for heavy cation removal from eco-system.     

New observations on scratch deformations of soda lime silica glass

In spite of the wealth of literature, the role of the scratching speed in affecting the material removal mechanism in soda lime silica (SLS) glass is yet to be comprehensively understood. Here we report the surface and sub‐surface deformation mechanisms of SLS glass scratched under three different normal loads of 5, 10 and 15 N at various speeds in the range of 100–1000 μm/s with a diamond indenter of ~ 200 μm tip radius. The results show that at any given applied normal load, the width, depth, wear volume of the scratch grooves and wear rate of the SLS glass decreased with an inverse power law dependence on the applied scratching speed. The surface damage also reduced with the increase in scratching speed. A new, simple model was developed to explain these observations. The significant contributions of the time of contact, the tensile stress behind the indenter and the shear stress active just underneath the indenter in governing the material removal mechanisms of the SLS glass were discussed.     

Crystal and molecular structure of a new biguanide metal complex, [Cu(AMNH)2]Cl2

The crystal structure of C₆H₁₆N₈O₂·CuCl₂, a biguanide metal complex, has been determined by X-ray diffraction data using MoK radiation. The compound crystallizes in the monoclinic space groupP2₁/a, witha=11.074(4),b=12.061(4),c=5.312(3)Å and=102.8(1)°.The structure was solved by direct methods and refined by full-matrix least-squares to a finalR value 0.037 with 1245 unique reflections. The complex molecule is centrosymmetric, with the Cu atom (0.5,0.5,0.5) on a crystallographic center of symmetry. The complex molecule is rhombic planar with a trans configuration.     

Synthesis of the anti-influenza agent (-)-oseltamivir free base and (-)-methyl 3-epi-shikimate

A new enantioselective synthesis of the anti-influenza agent (-)-oseltamivir free base (7.1% overall yield; 98% ee) and (-)-methyl 3-epi-shikimate (16% overall yield; 98% ee) has been described from readily available raw materials. Sharpless asymmetric epoxidation and diastereoselective Barbier allylation of an aldehyde are the key reactions employed in the incorporation of chirality, while the cyclohexene carboxylic ester core was constructed through a ring closing metathesis reaction.     

Dimethylaminoalkyl chalcogenolate palladium(II) complexes as an efficient copper- and phosphine-free catalyst for Sonogashira reaction

N,N-Dimethylaminoalkyl chalcogenolate Pd(II) complexes [PdCl(E^∩NMe₂)]_n has been investigated as a moisture/air-stable and robust catalyst for Sonogashira cross-coupling reaction in the absence of copper and phosphine ligand. The dimeric palladium(II) complex of selenium containing ligand shows the best catalytic activity as compared with monomeric and trimeric complexes. The variety of functional groups are tolerated under optimized catalytic systems and provide excellent yields of the products.     

Monte Carlo Simulation of Transient CSD in a Continuous Crystallizer under Stochastic Dispersion Effects

Monte Carlo simulation is a very powerful tool for simulation of transient and steady state crystal size distribution (CSD) in a continuous crystallizer under stochastic dispersion effects. In the present work, transient CSD in a continuous crystallizer has been reported when shape factor and growth rate dispersions conform to normal distribution. For the steady state run, the algorithm reported by Sen Gupta and Dutta elsewhere has been used to validate the results obtained in the present work when the steady state is reached.     

On circular designs

Summary A general method of analysis of circular designs (Das [3]) is suggested. Average efficiency factors of these designs have been tabulated.A-optimality of circular designs has been studied in comparison to group divisible incomplete block designs.     

Performance study of LaBr3:Ce detectors coupled to R2083 PM tube for energy and timing characteristics

Journal of Radioanalytical and Nuclear Chemistry - Performance of 1″?×?1″ LaBr3 (5% Ce) scintillator coupled to Hamamatsu R2083 PM Tube has been investigated for the...     

Synthesis, spectroscopic characterization and magnetic properties of homo- and heterodinuclear complexes of transition and non-transition metal ions with a new Schiff base ligand

Four homodinuclear complexes of Ni(II)-Ni(II), Cu(II)-Cu(II), Co(II)-Co(II) and Co(III)-Co(II) and five heterodinuclear complexes of Co(III)-Zn(II), Co(III)-Cu(II), Co(III)-Ni(II), Cu(II)-Zn(II) and Zn(II)-Cu(II) with the octadentate Schiff base compartmental ligand 1,8-N-bis(3-carboxy)disalicylidene-3,6-diazaoctane-1,8-diamine (H4fsatrien) have been synthesized. The complexes have been characterized with the help of elemental analyses, molecular weights, molar conductances, magnetic susceptibilities and spectroscopic (UV-vis, IR, ESR) data. Cryomagnetic data also helped to elucidate the structural features of the Cu(II) complexes.     

X-ray absorption spectroscopy and density functional theory studies of [(H3buea)FeIII-X]n- (X = S2-, O2-, OH-): comparison of bonding and hydrogen bonding in oxo and sulfido complexes

Iron L-edge, iron K-edge, and sulfur K-edge X-ray absorption spectroscopy was performed on a series of compounds [Fe(III)H(3)buea(X)](n-) (X = S(2-), O(2-), OH(-)). The experimentally determined electronic structures were used to correlate to density functional theory calculations. Calculations supported by the data were then used to compare the metal-ligand bonding and to evaluate the effects of H-bonding in Fe(III)(-)O vs Fe(III)(-)S complexes. It was found that the Fe(III)(-)O bond, while less covalent, is stronger than the Fe(III)(-)S bond. This dominantly reflects the larger ionic contribution to the Fe(III)(-)O bond. The H-bonding energy (for three H-bonds) was estimated to be -25 kcal/mol for the oxo as compared to -12 kcal/mol for the sulfide ligand. This difference is attributed to the larger charge density on the oxo ligand resulting from the lower covalency of the Fe-O bond. These results were extended to consider an Fe(IV)(-)O complex with the same ligand environment. It was found that hydrogen bonding to Fe(IV)(-)O is less energetically favorable than that to Fe(III)(-)O, which reflects the highly covalent nature of the Fe(IV)(-)O bond.