Polyesterification of aromatic dicarboxylic acids and bisphenols with tosyl chloride/dimethylformamide/pyridine promoted by the improvement of the difficult solubility of the activated diacids with lithium chloride

The solution polyesterification of dicarboxylic acids in pyridine, the activated intermediates of which were difficult to dissolve in tosyl chloride/dimethylformamide/pyridine, was investigated in the presence of lithium chloride. The solubility of the activated dicarboxylic acids was largely improved by the presence of the salt, and the polycondensation with bisphenols was greatly facilitated. The salt was more effectively added to a pyridine solution of dicarboxylic acids than to the activated dicarboxylic acids in pyridine. The favorable additive effect on the improved solubility was attributed to a lowered degree of association of the activated dicarboxylic acids, which led to distributions of the resulting oligomers from bisphenols at an earlier stage closer to the theoretical ones and yielded better polycondensation results. The reaction, which proceeded through favorable distributions of the co‐oligomers, produced copolymers of higher inherent viscosities and slightly block sequence distributions determined by NMR. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 2725–2733, 2004     

On practical metrology and chemical analysis: etalons and traceability systems

 National measurement systems are infrastructures to ensure, for each nation, a consistent and internationally recognised basis for measurement. Such complex systems have historical, technical, legal, organisational and institutional aspects to connect scientific metrology with practical measurements. Underlying any valid measurement is a chain of comparisons linking the measurement to an accepted standard. The ways the links are forged and the etalons (measurement standards) to which they connect are defining characteristics of all measurement systems. This is often referred to as traceability which aims at basing measurements in common measurement units – a key issue for the integration of quantitative chemical analysis with the evolving physical and engineering measurement systems. Adequate traceability and metrological control make possible new technical capabilities and new levels of quality assurance and confidence by users in the accuracy and integrity of quantitative analytical results. Traceability for chemical measurements is difficult to achieve and harder to demonstrate. The supply of appropriate etalons is critical to the development of metrology systems for chemical analysis. An approach is suggested that involves the development of networks of specialised reference laboratories able to make matrix-independent reference measurements on submitted samples, which may then be used as reference materials by an originating laboratory using its practical measurement procedures. Received: 31 July 1995 Accepted: 19 August 1995     

Diblock copolymers based on allyl methacrylate: Synthesis,characterization, and chemical modification

Different diblock copolymers constituted by one segment of a monomer supporting a reactive functional group, like allyl methacrylate (AMA), were synthesized by atom transfer radical polymerization (ATRP). Bromo‐terminated polymers, like polystyrene (PS), poly(methyl methacrylate) (PMMA), and poly(butyl acrylate) (PBA) were employed as macroinitiators to form the other blocks. Copolymerizations were carried out using copper chloride with N,N,N′,N″,N″‐pentamethyldiethylenetriamine (PMDETA) as the catalyst system in benzonitrile solution at 70 °C. At the early stage, the ATRP copolymerizations yielded well‐defined linear block copolymers. However, with the polymerization progress a change in the macromolecular architecture takes place due to the secondary reactions caused by the allylic groups, passing to a branched and/or star‐shaped structure until finally yielding gel at monomer conversion around 40% or higher. The block copolymers were characterized by means of size exclusion chromatography (SEC), ¹H NMR spectroscopy, and differential scanning calorimetry (DSC). In addition, one of these copolymers, specifically P(BA‐b‐AMA), was satisfactorily modified through osmylation reaction to obtain the subsequent amphiphilic diblock copolymer of P(BA‐b‐DHPMA), where DHPMA is 2,3‐dihydroxypropyl methacrylate; demonstrating the feasibility of side‐chain modification of the functional obtained copolymers. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 3538–3549, 2007     

High temperature annealing effect on structural and magnetic properties of Ti/Ni multilayers

High temperature annealing effect on structural and magnetic properties of Ti/Ni multilayer (ML) up to 600 °C have been studied and reported in this paper. Ti/Ni multilayer samples having constant layer thicknesses of 50 Å each are deposited on float glass and Si(1 1 1) substrates using electron-beam evaporation technique under ultra-high vacuum (UHV) conditions at room temperatures. The micro-structural parameters and their evolution with temperature for as-deposited as well as annealed multilayer samples up to 600 °C in a step of 100 °C for 1 h are determined by using X-ray diffraction (XRD) and grazing incidence X-ray reflectivity techniques. The X-ray diffraction pattern recorded at 300 °C annealed multilayer sample shows interesting structural transformation (from crystalline to amorphous) because of the solid-state reaction (SSR) and subsequent re-crystallization at higher temperatures of annealing, particularly at ≥400 °C due to the formation of TiNi₃ and Ti₂Ni alloy phases. Sample quality and surface morphology are examined by using atomic force microscopy (AFM) technique for both as-deposited as well as annealed multilayer samples. In addition to this, a temperature dependent dc resistivity measurement is also used to study the structural transformation and subsequent alloy phase formation due to annealing treatment. The corresponding magnetization behavior of multilayer samples after each stage of annealing has been investigated by using Magneto-Optical Kerr Effect (MOKE) technique and results are interpreted in terms of observed micro-structural changes.     

Series solution to the laser-ion interaction in a Raman-type configuration

The Raman interaction of a ultracold ion trapped with two travelling wave lasers is studied analytically with series solutions, in the absence of the rotating wave approximation (RWA) and without restrictions of both the Lamb-Dicke limit and the weak excitation regime. The comparison is made between our solutions and those obtained under the RWA in order to demonstrate the validity region of the RWA. As a practical example, the preparation of Schr?dinger-cat states is proposed beyond the weak excitation regime, using our calculations. Received 12 March 2001 and Received in final form 16 October 2001     

Ag-Bi高温超导线材转变温度的测量

介绍了 Bi系银包套高温超导线材的电阻温度特性 ,用测电阻和电磁感应两种方法分别测量了材料的超导转变温度 ,电磁感应法测量曲线上台阶的出现表明材料中 Bi(2 2 2 3)和 Bi(2 2 12 )两相的存在。     

Quantitative evaluation of two-dimensional dynamic deformations using digital holography

An optical system for the parallel evaluation of in- and out-of-plane dynamical deformations will be described. A double pulse laser with pulse separation in the microsecond range is used for the investigations. Two separate interferograms of an object under test, in its undeformed and deformed state, are recorded in a few microseconds. The object is illuminated from two different directions and imaged onto a CCD sensor. This produces two sensitivity vectors. The reference beams have different directions in order to produce two directional spatial carriers. The Fourier method is used for quantitative evaluation, and the measurements along different sensitivity vectors are separated in the Fourier domain. The phases of the two interferograms are obtained from the complex amplitudes and the two dimensional deformation is calculated from the phases. Experimental results are presented.     

Direct mass measurements of neutron-deficient 152Sm projectile fragments at the FRS-ESR facility

The FRS-ESR facility at GSI provides one of the most efficient methods for direct mass measurements. In the present experiment, exotic nuclei were produced via fragmentation of ¹⁵²Sm projectiles in a thick beryllium target at 500-600 MeV/u, separated in-flight with the fragment separator FRS, and injected into the storage-cooler ring ESR. Time-resolved Schottky Mass Spectrometry was applied for mass measurements of stored and electron-cooled bare and few-electron ions. 373 different nuclides were identified by means of the spectra of their revolution frequencies. Masses for 18 nuclides (⁸⁴Zr, ⁹²Ru, ⁹⁴Rh, ^107,108,110Sb, ^111,112,114I, ¹¹⁸Ba, ^122,123La, ¹²⁴Ce, ¹²⁷Pr, ¹²⁹Nd, ¹³²Pm, ¹³⁴Sm, ¹³⁷Eu) have been determined for the first time. Masses for ^111,112I and ¹¹³Xe have been obtained via known α-decay energies. The experiment and first results will be presented.     

Extension of the range of resonator scanning spectrometer into submillimeter band and some perspectives of its further developments

Extension of the working frequency of modern resonator spectrometers into submillimeter wave range is described. Experimental record of atmospheric absorption spectrum covering 45-370 GHz range is demonstrated for the first time, and measured water vapor J′_{ka′, kc′}-J_{ka, kc} = 5_1,5-4_2,2 at 325 GHz line parameters are presented. For the first time pressure lineshift for the 325-GHz water vapor line is measured. Further extension of working range is discussed. New estimations of physical limits of time needed for measurements of absorption in the whole Backward Wave Oscillator (BWO) range are given for phase continuous synthesizer regime. Basic schemes of fast broadband continuous phase synthesized sources are discussed. Verification of the previous measurements of water vapor 3_1,3-2_2,0 at 183 GHz line parameters is presented. Comparisons with ringdown resonator spectrometers are given.