Synthesis and characterization of new thermally stable poly(ester‐imide)s derived from 2,2′‐bis(4‐trimellitimidophenoxy)biphenyl and 2,2′‐bis(4‐trimellitimidophenoxy)‐1,1′‐binaphthyl and various aromatic dihydroxy compounds

A series of new alternating aromatic poly(ester‐imide)s were prepared by the polycondensation of the preformed imide ring‐containing diacids, 2,2′‐bis(4‐trimellitimidophenoxy)biphenyl (2a) and 2,2′‐bis(4‐trimellitimidophenoxy)‐1,1′‐binaphthyl (2b) with various aromatic dihydroxy compounds in the presence of pyridine and lithium chloride. A model compound (3) was also prepared by the reaction of 2b with phenol, its synthesis permitting an optimization of polymerization conditions. Poly(ester‐imides) were fully characterized by FTIR, UV‐vis and NMR spectroscopy. Both biphenylene‐ and binaphthylene‐based poly(ester‐imide)s exhibited excellent solubility in common organic solvents such as tetrahydrofuran, m‐cresol, pyridine and dichloromethane. However, binaphthylene‐based poly(ester‐imide)s were more soluble than those of biphenylene‐based polymers in highly polar organic solvents, including N‐methyl‐2‐pyrrolidone, N,N‐dimethylacetamide, N,N‐dimethylformamide and dimethyl sulfoxide. From differential scanning calorimetry thermograms, the polymers showed glass‐transition temperatures between 261 and 315 °C. Thermal behaviour of the polymers obtained was characterized by thermogravimetric analysis, and the 10 % weight loss temperatures of the poly(ester‐imide)s was in the range 449–491 °C in nitrogen. Furthermore, crystallinity of the polymers was estimated by means of wide‐angle X‐ray diffraction. The resultant poly(ester‐imide)s exhibited nearly an amorphous nature, except poly(ester‐imide)s derived from hydroquinone and 4,4′‐dihydroxybiphenyl. In general, polymers containing binaphthyl units showed higher thermal stability but lower crystallinity than polymers containing biphenyl units. Copyright © 2005 Society of Chemical Industry     

Continuous precipitation of calcium sulfate dihydrate from waste sulfuric acid and lime

Precipitation of calcium sulfate dihydrate, gypsum, from (i) a pure sulfuric acid/lime suspension and (ii) a waste sulfuric acid/lime suspension in a continuous pilot plant in the temperature range from 40 °C to 80 °C was studied. It was observed that in the case of waste sulfuric acid with a high content of Mg²⁺ and Fe²⁺ ions, several hours after the beginning of the precipitation, partial dissolution of the product and modification of the crystals from needle‐ and plate‐like to agglomerated structures occurred. It is suggested that the secondary changes occur due to the increased concentration of Mg²⁺ and Fe²⁺ ions in the reactor. Below 60 °C, and above 70 °C plate‐like and needle‐like single crystals respectively were formed. The mean size (d₅₀) of the crystals was found to increase with increasing temperature and decrease with the initial concentration of lime. Gypsum produced between 70 °C and 80 °C is suitable for further processing for construction plaster. In a precipitation process with pure sulfuric acid only single perfect needle‐like crystals occurred. Copyright © 2005 Society of Chemical Industry     

Synthesis and characterization of an interpenetrating polymer network composed of poly(methacrylic acid) and poly(vinyl alcohol)

Temperature and pH‐responsive interpenetrating polymer network (IPN) hydrogels, constructed with poly(methacrylic acid) (PMAA) and poly(vinyl alcohol) (PVA), by a sequential IPN method, were studied. The characterization of IPN hydrogels was investigated by Fourier‐transform infrared spectroscopy, differential scanning calorimetry (DSC) and swelling under various conditions. The IPN hydrogels exhibited relatively high swelling ratios, in the range 230–380 %, at 25 °C. The swelling ratios of the PMAA/PVA IPN hydrogels were pH and temperature dependent. DSC was used for the quantitative determination of the amounts of freezing and non‐freezing water. The amount of free water increased with increasing PMAA content in the IPN hydrogels. Copyright © 2004 Society of Chemical Industry     

Visual evaluation at scale of threshold to suprathreshold color difference

Visual evaluation experiments of color discrimination threshold and suprathreshold color‐difference comparison were carried out using CRT colors based on the psychophysical methods of interleaved staircase and constant stimuli, respectively. A large set of experimental data was generated ranged from threshold to large suprathreshold color difference at the five CIE color centers. The visual data were analyzed in detail for every observer at each visual scale to show the effect of color‐difference magnitude on the observer precision. The chromaticity ellipses from this study were compared with four previous published data, of CRT colors by Cui and Luo, and of surface colors by RIT‐DuPont, Cheung and Rigg, and Guan and Luo, to report the reproducibility of this kind of experiment using CRT colors and the variations between CRT and surface data, respectively. The present threshold data were also compared against the different suprathreshold data to show the effect of color‐difference scales. The visual results were further used to test the three advance color‐difference formulae, CMC, CIE94, and CIEDE2000, together with the basic CIELAB equation. In their original forms or with optimized K_L values, the CIEDE2000 outperformed others, followed by CMC, and with the CIELAB and CIE94 the poorest for predicting the combined dataset of all color centers in the present study. © 2005 Wiley Periodicals, Inc. Col Res Appl, 30, 198–208, 2005; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/col.20106     

An adaptive tracking problem for a family of retarded time-delay plants

Most of the existing switching control techniques are developed specifically for finite-dimensional linear time-invariant (LTI) systems. In many practical applications, however, it is essential to take time delay into consideration in the modelling as the control system can be highly sensitive to delay. In this paper, a multi-model switching control algorithm is proposed for retarded time-delay systems. It is assumed that the plant is represented by a family of known multi-input multi-output, observable, LTI models with multiple delays in the states, and that corresponding to each model in the known family, there exists a high-performance finite-dimensional LTI controller. In addition, it is supposed that a bound on the magnitude of the external inputs and disturbances is available. It is then shown that the proposed switching controller can stabilize the uncertain system, and that under some mild conditions, output tracking can be achieved in the given problem setting. Copyright © 2007 John Wiley & Sons, Ltd.     

Schwingfestigkeit von Schraube‐Mutter‐Verbindungen

High cycle fatigue of bolted connections Extensive tests regarding the influences on the fatigue of bolt‐nut‐connections of preloading with torsion, of preloading with yielding, of loading with superimposed bending and of the tested lot are processed. These influences are not yet known according to VDI 2230. New testing devices were designed for these tests, which allow a far less expensive operation and may easily be used for bolts of diameters up to M100 and testing frequencies up to 1000 Hz. The validity of fatigue resistance according to VDI 2230 is specified with respect to the test results. The determined influence of the tested lots is unexpectedly high. The manufacturing process of bolts should be improved to minimize this influence.     

Exchange and oxidation of CO on O-predosed Rh---Al2O3 and Rh---CeO2 catalysts

Exchange and oxidation of C¹⁶O were investigated at 450°C on ¹⁸O-predosed Rh and Pt catalysts supported on A1₂O₃, CeO₂ and CeO₂-Al₂O₃. In all cases, a rapid exchange of C¹⁶O with the surface can be observed. CO oxidation leads to C¹⁶O₂, C¹⁶O¹⁸O and C¹⁸O₂. Significant formation of C¹⁶O₂ is due to the relatively high ¹⁶O coverage in reaction resulting from the C¹⁶O exchange and from an exchange between O surface species and ¹⁶O internal atoms. Hydrogen is also formed via a water-gas shift reaction (CO + surface OH) in higher proportion on CeO₂-containing catalysts than on A1₂O₃. Chlorine inhibits all the reactions (exchange, oxidation and WGS) and particularly the internal exchange.