Anomalous elastic behaviour of Bi-Pb-Ag composites

Bi-Pb and Bi-Pb-Ag superconducting composites have been prepared by the solid state reaction method. After the usual characterization, ultrasonic longitudinal velocity and attenuation studies have been undertaken over a temperature range 80–300 K by the pulse transmission technique. In contrast to normal solids, the ultrasonic velocities of both the samples in the temperature range 200-100 K are found to decrease with decreasing temperature (softening), followed by a velocity maximum. The samples are also found to exhibit longitudinal attenuation peaks at TEMPERATURES = 260, 160 and 120 K. An attempt has also been made to verify whether the Wachtman's equations can theoretically explain the low-temperature behaviour of the Young's modulus of these materials. A qualitative explanation for both the phenomena of softening of velocity as well as the occurrence of attenuation peaks is given.     

Studies on the blends of cardanol-based epoxidized novolac resin and CTPB

Cardanol-based novolac-type phenolic resins were synthesized with different mole ratios of cardanol-to-formaldehyde, viz., 1:0.6, 1:0.7, and 1:0.8. These novolac resins were epoxidized with molar excess of epichlorohydrin at 120 °C in basic medium. The epoxidized novolac resins were, separately, blended with different weight ratios of carboxyl-terminated polybutadiene liquid rubber ranging between 0-25 wt% with an interval of 5 wt%. All the blends were cured at 150 °C with 40 wt% polyamide. The formation of various products during the curing of blend samples has been studied by Fourier-transform infra-red spectroscopic analysis. The tensile strength and elongation-at-break of the cured samples increased up to 15 wt% in the blend and decreased thereafter. This blend sample was also found to be most thermally stable system. The blend morphology, studied by scanning electron microscopy analysis, was finally correlated with the structural and property changes in the blends.     

Homogeneous isotopic exchange between nickel(II) and bis(diethyldithiocarbamato)nickel(II) complex

Isotopic exchange behaviour of bis(diethyldithio carbamate) nickel(II) complex with nickel(II) in chloroform and methanol medium was studied. The studies were carried out at different temperatures varying the concentration of both metal ion and the complex. The results show that the complex is labile in the kinetic sense. Increase in temperature increases the isotopic exchange rate. The increase in concentration also results in enhancement of the rate of reaction.     

One-Pot Convenient and High Yielding Synthesis of Dithiocarbamates

Summary. A convenient and high yielding method for the synthesis of diverse dithiocarbamates having various substituents including alkyl, aryl, heteroaryl, and alkylaryl at the thiol chain or at the amine chain or at both thiol and amine chains were developed by the one-pot reaction of mercaptans, amines, and bis(benzotriazolyl)methanethione in presence of amidine base under mild reaction conditions.     

Vaporization thermodynamics of thorium tetrafluoride

The thermal decomposition kinetics of Pr₂(SO₄)₃ to Pr₂O₂SO₄ have been studied by isothermal weight change determination. The reaction was found to obey a linear law up to α = 0.5; beyond α = 0.5 it could be described as a phase-boundary controlled process. A dependence of the activation energy upon the sample weight was observed. The changes in surface area and density which occur during the decomposition are also given.     

Microwave assisted low temperature synthesis of sodium zirconium phosphate (NaZr<Subscript>2</Subscript>P<Subscript>3</Subscript>O<Subscript>12</Subscript>)

Sodium zirconium phosphate [NaZr₂P₃O₁₂], a potential ceramic matrix for fixation of high level nuclear waste, was synthesized by heating the mixture of sodium carbonate [Na₂CO₃], zirconyl nitrate hydrate [ZrO(NO₃)₂·5H₂O] and ammonium dihydrogen phosphate [NH₄H₂PO₄] in air, in a resistance heated furnace and a microwave heating system respectively in the temperature range 450 to 650°C. The mixture heated for 1 h in a resistance furnace at 450°C yielded a poorly crystalline NaZr₂P₃O₁₂ [NZP]. Increasing the temperature to 650°C produced a highly crystalline product. The same mixture heated in a microwave oven at 450°C for 1 h however, yielded the most crystalline NZP.In an alternate method, the mixture of sodium dihydrogen phosphate (NaH₂PO₄), zirconium dioxide (ZrO₂) and diammonium hydrogen phosphate [(NH₄)₂HPO₄] heated in resistance furnace at 650°C for the same period did not react in air. It also did not yield the pure product at 450°C when heated in microwave assembly for 1 h.The authors thank the Board of Research in Nuclear Sciences (BRNS) of the Department of Atomic Energy (DAE) for the financial support for this work under the project No. 2000/37/19/BRNS/1959 dtd09-02-02.     

Enzymatic kinetic resolution of racemic 4-tetrahydropyranols by Candida rugosa lipase

Enzymatic kinetic resolution of (±)-hydroxytetrahydropyrans has been achieved for the first time by means of lipase-mediated transesterification to afford optically active (2S,4R)-tetrahydropyranyl acetates and (2R,4S)-tetrahydropyranols in excellent yields with high enantioselectivity. Absolute configurations of the tetrahydropyranyl acetates were assigned as (S) by chemical correlation.     

Alkynenitriles: chelation-controlled conjugate additions

[reaction: see text] Chelation between gamma-hydroxybutynenitrile and Grignard reagents triggers a particularly facile anionic conjugate addition reaction. Structurally diverse Grignard reagents add with equal efficiency, providing an intermediate anion that stereoselectively alkylates benzaldehyde in an overall addition-alkylation reaction.     

Recovery of americium from nitric acid solutions containing calcium by different co-precipitation methods

Recovery of americium from nitric acid solutions was studied by co-precipitation as hydroxide with various ions like calcium, ferric, nickel using sodium hydroxide and ammonium hydroxide. Studies were also carried out to recover americium using lanthanum fluoride and bismuth phosphate co-precipitation. All the methods are able to co-precipitate Am quantitatively. However, co-precipitation of Am with optimum concentration iron using ammonia is found to be better from nitric acid solutions containing large concentrations of calcium ions. Approximately 2 g of Am was recovered from 150 litres of solution batch wise using iron.     

Alkynenitriles: stereoselective chelation controlled conjugate addition-alkylations

Chelation-controlled conjugate addition of Grignard reagents to γ-hydroxyalkynenitriles stereoselectively generates tri- and tetra-substituted alkenenitriles. t-BuMgCl-initiated deprotonation of hydroxyalkynenitriles followed by addition of a second Grignard reagents triggers a facile conjugate addition leading to a cyclic magnesium chelate. Protonation of the chelate stereoselectively generates trisubstituted nitriles whereas the addition of t-BuLi causes conversion to an ‘ate’ complex that allows alkylation with aldehyde electrophiles. The chelation-controlled conjugate addition-alkylation generates tri- and tetra-substituted alkenenitriles that are otherwise difficult to synthesize.