13C CP MAS NMR of halogenated (Cl,Br, I) pharmaceuticals at ultrahigh magnetic fields

This work reports significantly improved spectral resolution of ¹³C CP MAS NMR spectra of chlorinated, brominated and iodinated solid organic compounds when such spectra are recorded at ultrahigh magnetic field strengths. The cause of this is the residual dipolar coupling between carbon atoms and quadrupolar halogen nuclides (chlorine‐35/37, bromine‐79/81 or iodine‐127), an effect inversely proportional to the magnetic field strength which declines in importance markedly at 21.1 T as compared to lower fields. In favorable cases, the fine structure observed can be used for spectral assignment, e.g. for Cl‐substituted aromatics where the substituted carbon as well as the ortho‐carbons show distinct doublets. The experimental results presented are supported by theoretical modeling and calculations. The improved spectral resolution in the studied systems and similar halogenated materials will be of particular interest and importance for polymorph identification, drug discovery and quality control in the pharmaceutical industry. Copyright © 2009 John Wiley & Sons, Ltd.     

Theoretical study of small silicon clusters on a graphite layer

In a series of recent experiments, the HOMO-LUMO energy gaps of small Si clusters deposited on a graphite substrate have been determined by Scanning Tunneling Microscopy (STM). The values obtained were found to be substantially smaller than the energy gaps of corresponding passivated clusters. This work considers dimensional reduction as a possible mechanism for a sizeable energy gap narrowing by the example of the system Si₅. The impact of the graphite substrate on the deposited species is investigated in the framework of a pseudocluster model. Received 30 November 2000     

Anomalous hysteretic phenomena in cyclotron resonance spectra of GaAs/AlGaAs quantum well under tilted magnetic fields of short pulse up to 150 T

We observed a new type of hysteresis in cyclotron resonance spectra of two-dimensional electron gas confined in GaAs/AlGaAs multi quantum wells when we applied high magnetic fields tilted from the growth direction. Pulsed high magnetic fields up to 150 T were generated by the single turn coil technique. We investigated in detail the condition for the occurrence of the hysteresis which is a disagreement between two traces in the up- and down-sweeps of the pulsed magnetic fields. The dependencies of the hysteresis on the wavelength, sweep rate of the fields and temperature has led to the conclusion that the hysteresis is due to inequilibrium states in the up-sweep of tilted magnetic fields. The relaxation time from inequilibrium to equilibrium states was revealed to be of the order of microsecond.     

电饭锅自动控温电路的设计和安装

本文紧紧抓住学生对“自动控温”这一普通现象的好奇 ,积极引导学生去探索和研究 ,使学生在掌握“自动控温”原理的基础上 ,按照自己的意愿和设想来设计一个电路并能动手组装和检验。     

Permeability control in electro‐sensitive microcapsules with immobilized ferroelectric liquid crystalline segments

Nylon‐polystyrene microcapsules with immobilized ferroelectric liquid crystalline segments were prepared, and permeability control of an encapsulated core material was investigated under an external electric field. A ferroelectric liquid crystal monomer possessing both mesogenicity and chirality responded effectively to the external electrical field. Permeation of the material (oxprenolol) contained in the inner aqueous core of the microcapsules was enhanced under a weak electric field (2 V). Furthermore, the permeability of oxprenolol did not depend on the external electric field in the absence of the ferroelectric liquid crystal segments. To clarify the controlled‐release mechanism of the core material, the light transmittance of the polymer membranes was quantitatively evaluated under an external electric field using a handmade polarized light transmittance apparatus. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 1749–1757, 2008     

Identification and quantification of polycarboxylates in detergent products using off-line size exclusion chromatography-nuclear magnetic resonance

The performance of many contemporary detergent products critically depends on polymers. Water-soluble polycarboxylates represent an important class of detergent polymers, and their quantitative assessment in detergent matrices stands as a considerable challenge. The presence of high levels of surfactants is a major complication, due to the strong tendency of surfactants to form micelles and to interact with the polymers. First, we addressed critical steps in the subsequent combined use of liquid extraction and off-line size exclusion chromatography-nuclear magnetic resonance (SEC-NMR) for identification and quantification of polycarboxylates in detergent products. Next, the different steps in the off-line SEC-NMR procedure were optimized with respect to precision and accuracy. This resulted in recoveries of more than 80% for maleic acid/acrylic acid copolymers; in detergent products a proportional bias of 30% is achieved. The method showed good precision with a relative standard deviation of within-laboratory reproducibility between 5% and 14%.     

Correlation Between Structure and Transport Properties of Polymeric Membranes for Immunoisolation

Laboratory-made asymmetric polyurethane membranes designed for immunoisolation were investigated. Two types of EK and ES membranes were prepared in different spinning conditions. The membrane structure was characterised by the skin pore radius measurements using differential scanning calorimetry (DSC). Diffusive transport properties of membranes were determined by in vitro method for albumin and creatinine. The scanning electron microscopy (SEM) was applied to study the morphology of membranes. It has been found that the DSC technique is a useful tool for the evaluation of pore radii in the skin layer for PU membranes. Calculated pore radii were in the range from 1.95 to 2.47 nm for the EK and ES types. A correlation between the skin pore radii and the transport properties was not found in this case of investigated membranes. However, the transport properties data can serve for the estimation of selectivity of membranes. Thus, the selectivity of membranes for solutes of various molecular size was estimated from the D _m/D _w ratio of diffusion coefficients for albumin and creatinine. The SEM micrographs reveal the finger-like internal structure of capillary membranes, as well as various skin thickness. This revised version was published online in July 2006 with corrections to the Cover Date.     

A Thermal And Structural Study on Lanthanum Hexacyanocobaltate(III) Pentahydrate. Part II

The thermal dehydration of La[Co(CN)₆]⋅5H₂O proceeded through at least three stages from the temperature range of30~230°C, and an abrupt mass loss occurred around 350°C and the perovskite type oxide,LaCoO₃ was obtained at 1000°C. After dehydration, the color of the anhydride changed from white to pale blue around 230°C and furthermore, the color changed to blue around 290°C. These color changes were discussed on the basis of the changes of coordination structures around Co ions. In La[Co(CN)₆]⋅5H₂O, Co³⁺ ions lie at the center of the O_h crystal field consisted of six CN^– ions. However, in the pale blue specimen, Co³⁺ ions were situated in the center of D_4h crystal field which was distorted the O_h one by lengthening of the trans CN^– ions along z-axis. In the blue specimen, Co³⁺ ions were reduced to Co²⁺ ions which were situated in the T_d crystal field formed by four CN^–ions as [Co(CN)₄]^2–. This revised version was published online in July 2006 with corrections to the Cover Date.     

电阻环法模拟测量电子束流的大小和位置

本文介绍了通过测量束流在输运管壁上形成的感应电流，来确定直线感应加速器束流大小、位置的一种方法。实验证明，这种测量方法不会影响电子束在管道中的传输，且测量精度高，装置简单，并可装在真空系统的外面，便于维修。     

Spin fluctuation effects in substituted CeRu2Si2 and YbPd2Si2 alloys

Effects of chemical substitution in CeRu₂Si₂, a well-studied heavy fermion system and YbPd₂Si₂ have been investigated through magnetic susceptibility and x-ray diffraction in the systems CeRu _x Si₂, CeRu_2−x Os _x Si₂, CeRu₂Si_2−x Ge _x and YbPd₂Si_2−x Ge _x . Replacing silicon by germanium generates normal chemical pressure effect, namely, Ce and Yb atoms in CeRu₂Si₂ and YbPd₂Si₂ became more and less magnetic respectively. With increasing Ge concentration, CeRu₂Si_2−x Ge _x exhibits larger susceptibility at low temperature, goes to an antiferromagnetic state and finally becomes ferromagnetic. In YbPd₂Si_2−x Ge _x , increasing Ge concentration drives Yb atoms to more divalent state. Electronic effects are more pronounced in CeRu_2−x Os _x Si₂ though CeRu₂Si₂ and CeOs₂Si₂ have very nearly the same lattice parameters. It is conjectured that CeRu₂Si_2−x Ge _x may be the first Ce-based heavy fermion having a magnetic ground state. The authors felicitate Prof. D S Kothari on his eightieth birthday and dedicate this paper to him on this occasion.