Further utilisation of 2-naphthol esters: polarographic determination of phosphatase and arylsulphatase activities

Summary The Polarographic method of the determination of alkaline and acid phosphatases and arylsulphatases using esters of 2-naphthol has been elaborated. The enzymatically released 2-naphthol is nitrosated and the nitrosation product (1-nitroso-2-naphthol) is reduced on the mercury drop-electrode with the production of a well-developed four-electron wave. The method was applied for the determination of the enzymatic activity of tissue homogenates and commercial enzyme preparations.

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Weitere Anwendbarkeit von 2-Naphthol-Estern : Polarographische Bestimmung der Aktivität von Phosphatase und Arvlsulphatase

Zusammenfassung Es wurde eine Methode zur polarographischen Bestimmung der Aktivität der alkalischen und sauren Phosphatasen und Arylsulphatasen bei Benützung der 2-Naphthol-Ester ausgearbeitet. Das durch enzymatische Hydrolyse freigesetzte 2-Naphthol wird nitrosiert und das Nitrosierungsprodukt (1-Nitroso-2-Naphthol) auf der Quecksilber-Tropfelektrode bei Entstehung einer gut entwickelten Welle reduziert. Diese Methode wurde bei Bestimmung der enzymatischen Aktivität in Gewebehomogenaten wie auch in enzymatischen Handelspräparaten verwendet.

     

Determination of organophosphorus insecticides in edible oils and fats by splitless injection of the oil into a gas chromatograph (injector-internal headspace analysis)

Direct injection of oil or fat into a moderately heated injector enables performance of a kind of head-space technique in, the injector: oil or fat is diluted 11 with acetone and injected into a vaporizing chamber at 200° C. Components, for example organophosphorus insecticides, evaporate from the oil film on the insert wall and are transferred into the column in the splitless mode; the oil slowly flows along the wall to the bottom of the insert and is retained there in a kind of a bag. Using a flame photometric detector, detection limits are below 10 g/kg.

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Bestimmung von Phosphorsäureester-Insektiziden in Speiseölen und -fetten durch splitlose Einspritzung des Öls in den Gaschromatographen (Injektor-interne Head-spaceanalyse)

Zusammenfassung Direkte Einspritzung von Öl oder Fett in einen mäßig heißen Injektor des Gaschromatographen erlaubt eine Art Headspacetechnik im Verdampfungsinjektor: Öl oder Fett wird 11 mit Aceton verdünnt und bei 200 °C eingespritzt. Die Komponenten, z. B. Phosphorsäureester-Insektizide, verdampfen aus dem Ölfilm auf der Röhrchenwand und werden splitlos in die Säule übertragen. Das Öl fließt langsam der Wand entlang nach unten und wird in einer Art Tasche aufgefangen. Mit flammenphotometrischer Detektion liegt die Nachweisgrenze unter 10 g/kg.

     

Influence of flexible segment length on the phase structure and properties of poly(hexamethylene 2,5-furandicarboxylate)-block-biopolytetrahydrofuran copolymers

Two series of biobased poly(ether-ester)s comprised of poly(hexamethylene 2,5-furandicarboxylate) (PHF) as the rigid segments and biopolytetrahydrofuran (pTHF) with different molecular masses (1000 and 2000 g/mol) as the flexible segments were synthesized employing polycondensation in the molten state. The study mainly focuses on comparing these two series in terms of the length of the flexible segment. The content of pTHF segments in the copolymer chains varied from 25 to 75 wt.%. The molecular structure and composition, phase structure, and thermal and mechanical properties were characterized by nuclear magnetic resonance (¹H NMR) and Fourier-transformed infrared (FTIR) spectroscopies, differential scanning calorimetry (DSC), dynamic mechanical thermal analysis (DMTA), and positron annihilation lifetime spectroscopy (PALS). In addition, mechanical performance and thermo-oxidative and thermal stability have been investigated. Moreover, cyclic tensile properties were studied to evaluate the elastic properties. ¹H NMR and FTIR spectroscopies demonstrate that the syntheses were correctly carried out, which made it possible to obtain the desired compositions of the block copolymers with high molecular masses. The decrease in T_m1, T_c1, and X_cPHF values was visible, along with the increase in the flexible segment content. Moreover, the characteristic properties measured by PALS and the values of temperatures designated from TGA (inert and oxidizing atmosphere) did not vary between copolymer series PHF-b-F-pTHF1000 and PHF-b-F-pTHF2000. In turn, along with an increase in flexible segment content and the length of the pTHF, the values of tensile modulus, stress at break, and hardness decrease, while the value of elongation at break increases.     

Bemessung eines Stützbauwerks nach Eurocode — Teil 2: Erdbebenbemessung

Dieser Beitrag behandelt den Erdbebennachweis für die Bemessung von Gewichtsmauern aus Beton und Stahlbeton nach Eurocode 2 (EN 1992‐x), Eurocode 7 (EN 1997‐1) und Eurocode 8 (EN 1998‐x) anhand eines durchgerechneten Beispiels. Design of concrete retaining structures according to Eurocode standards — Part 2: Earth quake design. This contribution treats the design of concrete retaining structures under earth quake impact based on Eurocode 2 (EN 1992‐x), Eurocode 7 (EN 1997‐1) and Eurocode 8 (EN 1998‐x) by means of an application example.     

Model based control of a liquid swelling constrained batch reactor subject to recipe uncertainties

This work presents the application of nonlinear model predictive control (NMPC) to a simulated industrial batch reactor subject to safety constraint due to reactor level swelling, which can occur with relatively fast dynamics. Uncertainties in the implementation of recipes in batch process operation are of significant industrial relevance. The paper describes a novel control-relevant formulation of the excessive liquid rise problem for a two-phase batch reactor subject to recipe uncertainties. The control simulations are carried out using a dedicated NMPC and optimization software toolbox OptCon which implements efficient numerical algorithms. The open-loop optimal control problem is computed using the multiple-shooting technique and the arising nonlinear programming problem is solved using a sequential quadratic programming (SQP) algorithm tailored for large-scale problems, based on the freeware optimization environment HQP. The fast response of the NMPC controller is guaranteed by the initial value embedding and real-time iteration technologies. It is concluded that the OptCon implementation allows small sampling times and the controller is able to maintain safe and optimal operation conditions, with good control performance despite significant uncertainties in the implementation of the batch recipe.     

FE analyses and tests in support of Wendelstein 7-X trim coil development

The paper presents an overview of the finite element (FE) analyses on the trim coils (TCs) and tests performed at IPP, and focuses on some specific aspects of the TC assembly. Global FE models (GM) of two types of TCs predicted the coil deformations and reaction forces on the supports. Dead weight, temperature rise during operation up to 80 °C, electromagnetic loads of 19 field configurations, and outer vessel (OV) deformations have been taken into account. In addition, local models were created for the critical winding pack (WP) regions as well as for each support clamp, and were analyzed with boundary conditions determined by the GM. The detailed WP sub-models were developed to verify the insulation strength against local stresses. The simulations were supported by various mechanical tests under static and cyclic loads. Aim of these experiments was to determine the time dependent behavior of the silicone rubber pads which are used as interfaces between TC and supports, and to check and optimize the assembly tools as well as procedures for the TCs and their supports.     

Deduction of the He–Fe interaction potential in eV-range from experimental data by computer simulation in grazing ion-surface scattering: Row-model

In glancing-angle scattering of keV-ions from a crystal surface, the ion reflection takes place in the eV-part of the interaction potentials. The elastic interactions are determined by the energy transverse to atomic rows, which can be of the order of 10 eV. A row-model using averaged potentials according to the Lindhard cylindrical potential has been developed using step-by-step integration of Newton's equations of motion. Previously [D. Danailov, K. Gärtner, A. Caro, Nucl. Instr. and Meth. B 153 (1999) 191; presented on COSIRES, Okayama, 1998] we reported that zig–zag trajectories within surface channels and the corresponding multimode azimuthal angular distributions of reflected ions are very sensitive to the interaction potential used in the simulation. Here we simulate the scattering of 15 keV He-atoms from Fe(1 0 0) surfaces at different angles of incidence comparable with previously published experimental results [D. Danailov, T. Igel, R. Pfandzelter, H. Winter, Nucl. Instr. and Meth. B 164–165 (2000) 583]. Our results show that for interaction energies below about 4 eV the well-known “universal” potential works well. However, for energies between 4 and 13 eV the “individual” He–Fe potential (D. Danailov, K. Gärtner, A. Caro, Nucl. Instr. and Meth. B 153 (1999) 191; presented on COSIRES, Okayama, 1998) gives a better agreement with the experimental data. For interaction energies above 13 eV both potentials are similar. We have constructed a mixed He–Fe potential, which describes the experimental observations well. The row-model enables us to deduce the He–Fe interaction potential in the eV-range. In addition, a shift in the experimental angular spectra compared with the calculated spectra indicates that the atomistic rows undergo an elastic horizontal bend due to the scattering and an order of magnitude smaller vertical displacement.