R.F. (280 MHz) EPR imaging of extended samples: Apparatus and preliminary results

This paper presents the preliminary results obtained using an Electron Paramagnetic Resonance imaging apparatus operating at 280 MHz. The acquisition technique and the procedure used to obtain the spin density spatial localization are presented and specimen images of extended samples are given. The accuracy of the images and the spatial resolution are also discussed.     

Side‐chain crystallization behavior of graft copolymers consisting of an amorphous main chain and crystalline side chains. II. Poly(n‐hexyl methacrylate)‐graft‐poly(ethylene glycol)

The phase behavior and crystallization of graft copolymers consisting of poly(n‐hexyl methacrylate) (PHMA) as an amorphous main chain and poly(ethylene glycol) (PEG) as crystallizable side chains (HMAx with 15 ≤ x ≤ 73, where x represents the weight percentage of PEG) were investigated. Small‐angle X‐ray scattering profiles measured above the melting temperature of PEG suggested that a microdomain structure with segregated PHMA and PEG domains was formed in HMA40 and HMA46. This phase behavior was qualitatively described by a calculated phase diagram based on the mean‐field theory. Because of the segregation of PEG into microdomains, the crystallization temperature of the PEG side chains in HMAx was higher than that in poly(methyl acrylate)‐graft‐poly(ethylene glycol) having a similar value of x, which was considered to be in a disordered state above the melting temperature. In HMAx with x ≤ 40, PEG crystallization was strongly restricted, probably because the PEG microdomains were isolated in the PHMA matrix. As a result, the growth of PEG spherulite was not observed because the PEG crystallization occurred after vitrification of the PHMA segregated domains. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 45: 129–137, 2007     

Synthesis of silicon nitride based ceramic nanoparticles by the pyrolysis of silazane block copolymer micelles

Diblock copolymer poly(1,1,3,N,N′‐pentamethyl‐3‐vinylcyclodisilazane)‐block‐polystyrene (polyVSA‐b‐polySt) and triblock copolymer poly(1,1,3,N,N′‐pentamethyl‐3‐vinylcyclodisilazane)‐block‐polystyrene‐block‐poly(1,1,3,N,N′‐pentamethyl‐3‐vinylcyclodisilazane) (polyVSA‐b‐polySt‐b‐polyVSA), consisting of silazane and nonsilazane segments, were prepared by the living anionic polymerization of 1,1,3,N,N′‐pentamethyl‐3‐vinylcyclodisilazane and styrene. PolyVSA‐b‐polySt formed micelles having a poly(1,1,3,N,N′‐pentamethyl‐3‐vinylcyclodisilazane) (polyVSA) core in N,N‐dimethylformamide, whereas polyVSA‐b‐polySt and polyVSA‐b‐polySt‐b‐polyVSA formed micelles having a polyVSA shell in n‐heptane. The micelles with a polyVSA core were core‐crosslinked by UV irradiation in the presence of diethoxyacetophenone as a photosensitizer, and the micelles with a polyVSA shell were shell‐crosslinked by UV irradiation in the presence of diethoxyacetophenone and 1,6‐hexanedithiol. These crosslinked micelles were pyrolyzed at 600 °C in N₂ to give spherical ceramic particles. The pyrolysis process was examined by thermogravimetry and thermogravimetry/mass spectrometry. The morphologies of the particles were analyzed by atomic force microscopy and transmission electron microscopy. The chemical composition of the pyrolysis products was analyzed by X‐ray fluorescence spectroscopy and Raman scattering spectroscopy. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 4696–4707, 2006     

A new on-line sample preparation system for the liquid chromatography/time-of-flight mass spectrometry simultaneous analysis of pesticides in river water.

Current on-line solid-phase extraction methods combined with HPLC for shortening the clean-up operation are not suitable for simultaneously detecting compounds that have a wide variety of hydrophobicities. To solve these problems, we designed a new on-line sample preparation system. The system consists of an eluting pump, a mixing TEE connector, a 10-port 2-position valve and a solid-phase extraction precolumn. The eluate from the precolumn is diluted with a weak solvent from the HPLC at the TEE connection to load low hydrophobic compounds onto the analytical column. The proposed on-line sample preparation system was successfully applied to the simultaneous analysis of 21 pesticides in river water using LC/TOF-MS. In this method, the recoveries from river water samples were 67 to 126% (mean 83%), the reproducibility (CV%) was in the range from 1.1 to 11% (mean 5.6%), the calibration curve was linear in the range from 1 ppb to 500 ppb (r > 0.999) and the detection limits (S/N = 3) were in the range from 0.0034 ppb (daimuron) to 3.3 ppb (oxine-copper).     

Gasdynamische Untersuchung des Jouleschen Überströmversuches

Zusammenfassung Es wird die zeitabhängige Strömung beim Ausgleichsvorgang zwischen zwei endlichen Behältern untersucht. Den Überlegungen wird eine eindimensionale, reibungsfreie und quasistationäre Strömung zugrunde gelegt. Während bei überkritischer Strömung eine analytische Lösung möglich ist, wird das Problem bei unterkritischer Strömung numerisch gelöst.Dem Druckausgleich zwischen den beiden Behältern folgt ein isobarer Wärme- und Massenaustausch, bis sich das thermodynamische Gleichgewicht eingestellt hat.

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Gasdynamical investigation of Joule's overflow experiment

The time-dependent flow of an exchange process between two big insulated tanks is considered. The problem is treated on the basis of a one-dimensional, inviscid and quasi-steady flow. An analytical solution is obtained for supercritical flow, while for subcritical flow the problem is solved numerically.After the pressure-equilibrium between the two-tanks an isobar heat and mass exchange follows, until the thermodynamic equilibrium is reached.

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Formelzeichen a Schallgechwindigkeit - A engster Querschnitt - c Geschwindigkeit - c _p spezifische Wärme bei konstantem Druck - c _v spezifische Wärme bei konstantem Volumen - e innere Energie - i Enthalpie - m Masse - M Machzahl - p Druck - spezielle Gaskonstante - s Stromlinie, spezifische Entropie - t dimensionsbehaftete Zeit - T Temperatur - V Volumen - Konstante - Abkürzung - Volumenverhältnis - Verhältnis der spezifischen Wärmen - Dichte - dimensionslose Zeit Indizes 0 Zustand zur Zeitt=0 - 1 Zustand im Überdruckbehälter - 2 Zustand im Überströmbehälter - * Zustand im engsten Querschnitt - K kritisch - M Zustand bei Druckausgleich - E Endzustand bei Temperaturausgleich Herrn Prof. Dr. B. Schmidt in Dankbarkeit zum 60. Geburtstag gewidmet     

Eine direkt formulierte lineare Theorie für viskoelastische Platten und Schalen

Übersicht Eine Möglichkeit der Entwicklung einer allgemeinen Theorie für Platten und Schalen besteht in der Modellierung des Flächentragwerks durch ein zweidimensionales deformierbares Kontimmm und der direkten Ableitung der kinematischen Beziehungen, der Bewegungsgleichungen und der konstitutiveu Gleichungen. Eine so erhaltene Theorie ist mathematisch und physikalisch widerspruchsfrei, jedoch ist es für ihre Anwendung notwendig, die sogenannten Ersatzeigenschaften zu ermitteln. Im Beitrag wird eine geometrisch und physikalisch lineare Theorie behandelt. Jeder Punkt des Kontinuums ist ein infinitesimal kleiner Starrkörper mit nur 5 Freiheitsgraden (3 Translationen, 2 Rotationen). Bei Annahme dieser Einschränkungen gelingt es, eine Theorie direkt abzuleiten, wobei alle Ersatzeigenschaften des Flächentragwerks bestimmt werden können. Im Beitrag werden die Möglichkeiten der allgemeinen Theorie am Beispiel isotropen viskoelastischen Materials mit über die Dicke veränderlichen Eigenschaften gezeigt. Die Theorie schließt die Betrachtung mehrschichtiger Flächentragwerke ein.

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A directly formulated linear theory of viscoelastic plates and shells

Summary One kind to develop a general theory for plates and shells is the modelling of the structure as a two-dimensional deformable continuum and the direct approach to the kinematical relations, equations of motion and constitutive equations. Such a theory is physically and mathematically correct. For the application of such directly formulated theories it is nessecery to identify the so-called effective properties. In the paper the theory is formulated for geometrical and physical linearity. Each point of the continuum is an infinitesimal small rigid body with only 5 degrees of freedom (3 translations, 2 rotations). For such a kinematical assumption it is possible to develop a direct theory and to determinate all effective properties of the structure. The paper demonstrates the possibilities of the general theory for an isotropic viscoelastic plate with material properties varying over the thickness. The theory includes also the analysis of multilayered plates and shells.

     

Plane contact problems for a periodic two-layered elastic composite

Summary This paper deals with the two-dimensional static punch problems in the presence of friction for a periodically layered half-space. Within the framework of the homogenized model of linear elasticity with microlocal parameters [8–11] the exact solutions of the considered problems are obtained. The case of the indentation of the composite body by a rigid rectangular punch has been discussed in detail.

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Ebene Kontaktprobleme für ein periodisches elastisches Zweischichten-Komposit

Übersicht In dieser Arbeit wird das zweidimensionale statische Stempelproblem mit Reibung für einen periodisch geschichteten Halbraum betrachtet. Im Rahmen eines Homogenisierungsmodells der linearen Elastizitätstheorie mit mikropolaren Parametern werden die exakten Lösungen der betrachteten Probleme gewonnen. Im Detail wird das Eindringen eines rechteckigen starren Stempels behandelt.

     

4-Amino-imidazole durchThorpe-Cyclisierung

The alkylation of arylaminomethylenecyanamides1 or cyano-imidothiocarbamates2 with -halogen carbonyl compounds followed by base catalysed cyclization yields substituted 4-amino-imidazoles4. Imidazo[4,5-d]pyrimidones5, 6 and imidazo[4,5-b]pyridines7 can be obtained from4.     

The electrocapillarity of polyacrylates

Summary The electrocapillary properties of polyacrylic acid have been studied by two methods. Exploratory measurements have been made of the effect of the polymer on the differential capacity of a mercury drop in 0.1 m sodium perchlorate. They showed that the polymer was strongly adsorbed over a wide range of potentials but that it did not appear to form a monolayer. The surface excess of polymer obtained from drop weight data showed a maximum at very low concentrations and then a decline at higher concentrations. The bulk of the work was carried out by making surface tension measurements, using a sessile mercury drop, in solutions of a fraction of polyacrylic acid (mol. wt. 7.02×10⁴) in potassium chloride at 0.01, 0.1, 0.2, and 0.5 m at 25°C.The data have been used to evaluate the surface excesses of the polymer and of the inorganic ions. The distribution of K⁺ and Cl^– in the electrical double layer and the contact adsorption of Cl^– on the mercury were very little affected by the presence of the polymer. The surface excess of polymer was always found to be greatest at low concentrations, to decrease steeply at first as the concentration was increased and then to decrease more slowly at higher concentrations.Possible explanations of this behaviour are discussed and it is concluded that the rapid decrease is a consequence of molecular weight dispersion and the stronger adsorption of high molecular weight polymer. The slow decrease in surface excess at higher concentrations may be a result of configurational changes of the polymer molecules.Surface pressure data show that, despite this decrease in the surface excess, the surface coverage reaches a high level at very low polymer concentrations and then continues to increase slowly as the concentration of polymer is increased. This apparent contradiction is due to changes in configuration of the adsorbed polymer molecules. At higher bulk concentrations the chain configurations are more compact and each adsorbed molecule makes more contacts with and so occupies a greater area of the mercury surface than at low concentrations.The conclusion is reached that the surface excess of polymer is mostly contained in a layer probably more than 1000 Å thick. It consists of a concentrated and entangled mass of polymer chains. Relatively few of these chains are in contact with the mercury at any istant. The concentration in this surface layer decreases steadily with increasing distance from the mercury surface and it merges without discontinuity into the bulk solution.With 10 figures in 22 details