Preparation, characterization and thermolysis of metal nitrate complexes with 4,4’-bipyridine

Two bis(bipyridine) polymeric metal nitrate complexes with 4,4’-bipyridine of simple formula like [M(bipy)₂](NO₃)2⋅xH₂O (where M=Co, Ni and Cu; x=4, 2 and 0, respectively) have been prepared and characterized. Their thermal decomposition has been undertaken using simultaneous TG-DTG-DTA and DSC in nitrogen atmosphere and non-isothermal TG in air atmosphere. Isothermal TG has been performed at decomposition temperature range of the complexes to evaluate the kinetics of decomposition by applying model-fitting as well as isoconversional method. Possible mechanistic pathways have also been proposed for the thermolysis. Ignition delay measurements have been carried out to investigate the response of these complexes under the condition of rapid heating.     

Fingerprints of Phalaenopsis Tissues in Growth and Spike Induction Periods—A Solid‐state 13C NMR Approach

Solid‐state Nuclear Magnetic Resonance (ss‐NMR) ¹³C single‐pulse excitation spectroscopy in combination with the magic‐angle spinning (MAS) technique was applied to a series of Phalaenopsis tissues, including the leaf, sheath, stem, and root, at different growth and spiking periods. Compared with{¹H}/¹³C cross‐polarization MAS spectra, the ¹³C single‐pulse excitation MAS spectra displayed very distinct spectral patterns, recognizable as fingerprints of the tissues studied. ¹Here, we demonstrate that solid‐state ¹³C single‐pulse excitation NMR spectroscopy provides a direct and robust analytical tool for studying the various tissues of Phalaenopsis in different growth and spiking induction periods.     

Rotor-synchronized two-dimensional 13C CP/MAS NMR studies of the orientational order of polymers 2. Melt-extruded poly(ethylene terephthalate) fibers

Determination of the orientational order of morphological components in polyethylene terephthalate (PET) is sought through quantitative application of two-dimensional rotor synchronized magic angle spinning (ROSMAS) ¹³C NMR technique. Previous study in our laboratories had established a procedure for resolution of the carbonyl carbon (CA) and glycol ethylene carbon (GE) resonances into those corresponding to four morphological components.¹ Due to paucity of sidebands in the GE resonances, the focus has been on the CA resonances in this attempt to obtain orientation distributions. A set of PET fibers possessing a broad range of crystalline and orientational order has been used to infer the meaning of NMR-based orientation measurements vis-a-vis other techniques. A surprising finding of this study is the observation that the orientational orders of the broad component in the ¹³C CP/MAS spectrum and the narrow component are very similar in these fibers. ©1995 John Wiley & Sons, Inc.     

A solid-state NMR application of the anomeric effect in carbohydrates: galactosamine, glucosamine, and N-acetyl-glucosamine

Simple 2D 13C/15N heteronuclear correlation solid-state NMR spectroscopy was implemented to resolve the 15N resonances of the alpha and beta anomers of three amino monosaccharides: galactosamine (GalN), glucosamine hydrochloride (GlcN), and N-acetyl-glucosamine (GlcNAc) labeled specifically with 13C1/15N spin pairs. Although the 15N resonances could not be distinguished in normal 1D spectra, they were well resolved in 2D double CP/MAS correlation spectra by taking advantage of the 13C spectral resolution. The alpha and beta resonances shifted apart by 3-5 ppm in their 13C chemical shifts, and differed by 1-2 ppm in the extended 15N dimension. Aside from this, the detection of other 13C/15N correlations over short distances was also achieved arising from the C2, C3 and CO carbons present in natural abundance. 2D double CP/MAS chemical shift correlation NMR spectroscopy is a simple and powerful technique to characterize the anomeric effect of amino monosaccharides. Applications of the 2D method reveal well-resolved 15N and 13C chemical shifts might be useful for structural determination on carbohydrates of biological significance, such as glycopeptide or glycolipids.     

Solid-state 13C NMR characterization of molecular orientation of hot drawn nylon 6

Two-dimensional cross polarization (CP), magic angle spinning (MAS) rotor synchronization NMR spectroscopy has been used to determine quantitatively the molecular orientational distribution function on hot-drawn Nylon 6. Both films and fibers are studied that had been thermally deformed at temperature above T_g, from 60 to 175°C at draw ratios in the range of 1-5.5. In the two-dimensional NMR spectrum, the sidebands that intrinsically originate from the chemical shift anisotropy reveal the degree of molecular orientational order. No preferential orientational order is detected for the sample without thermal deformation, and the highest degree of order is observed for samples which have been hot drawn above T_g at ratios ca. 5. Based on the aggregate model the maximum achievable order parameters are determined. © 1994 John Wiley & Sons, Inc.     

直接键连原子间的NMR偶合常数的自然杂化轨道研究V.~(13)C-~(13)C和~(13)C-~(31)P核自旋偶合常数~1J_(CC)和~1J_(CP)

在前文工作的基础上，结合ＭＮＤＯ／ＥＨＭＯ分子轨道方法和自然杂化轨道方法，具体计算了ＣＣ键和ＣＰ键的核自旋偶合常数．计算结果表明，１ＪＣＣ和１ＪＣＰ主要由成键原子的轨道杂化作用和键极性这两种结构因素所决定．为从简单价键理论角度解释和计算１ＪＣＣ和１ＪＣＰ值提供了简便直观的方法．     

Thermal conductivity of NbSe3

The thermal conductivity, κ, of NbSe₃ has been measured by novel self-heating techniques that allowed the electric field dependence of κ to also be measured. Measurements were made from 35 K to room temperature. Above the charge density wave transitions, the phonon thermal conductivity is 4–7 times the electron thermal conductivity, and it rises smoothly below the transitions, indicating that phonon-phonon scattering predominates. Phonon mean free parths have been estimated at 187 A° at 60 K and 60 A° at 150 K. No clear anomalies were observed at the phase transitions, giving upper limits to changes in the phonon mean free path. No field dependence of κ was observed.     

Iterations of anti-selfdual Lagrangians and applications to Hamiltonian systems and multiparameter gradient flows

Anti-selfdual Lagrangians on a state space lift to path space provided one adds a suitable selfdual boundary Lagrangian. This process can be iterated by considering the path space as a new state space for the newly obtained anti-selfdual Lagrangian. We give here two applications for these remarkable permanence properties. In the first, we establish for certain convex–concave Hamiltonians on a–possibly infinite dimensional–symplectic space H ², the existence of a solution for the Hamiltonian system that connects in a given time T > 0, two Lagrangian submanifolds. Another application deals with the construction of multiparameter flows, including those generated by vector fields that represent superpositions of skew-adjoint operators with gradients of convex potentials. Our methods are based on the new variational calculus for anti-selfdual Lagrangians developed in [5–7].     

Inverse problems with partial data for a Dirac system: A Carleman estimate approach

We prove that the material parameters in a Dirac system with magnetic and electric potentials are uniquely determined by measurements made on a possibly small subset of the boundary. The proof is based on a combination of Carleman estimates for first and second order systems, and involves a reduction of the boundary measurements to the second order case. For this reduction a certain amount of decoupling is required. To effectively make use of the decoupling, the Carleman estimates are established for coefficients which may become singular in the asymptotic limit.