Photometrische Bestimmung von Nitrit mit Rivanol

Zusammenfassung In der vorliegenden Arbeit wurden die Reaktionsbedingungen zur colorimetrischen Bestimmung von Nitrit mit Rivanol untersucht. Die Bestimmung ist einfach durchzuführen und für Nitrit weitgehend selektiv. Die Farbenintensität ist von der Konzentration der salpetriger Säure linear abhängig.     

Chemie der Seltenerdmetalle, 15. Mitt.: Chlortartratkomplexe der Seltenerdmetalle des Typs LnH2TCl·xH2O

Zusammenfassung Es wurden Komplexe des Typs YH₂ TCl·2H₂O, LaH₂ TCl·3H₂O und CeH₂ TCl·3H₂O isoliert. Die Individualität der Verbindungen wurde mit Hilfe der Thermoanalyse, IR-Absorptionsspektren und Röntgenstreuung geklärt.Complexes of the types YH₂ TCl·2H₂O, LaH₂ TCl·3H₂O and CeH₂ TCl·3H₂O were isolated, and the compounds characterized by thermogravimetric analysis, I. R. spectroscopy and X-ray diffraction.Mit 3 Abbildungen Ln=Y, La, Ce; H₄ T=C₄H₆O₆.     

Photochemistry of condensed isoxazolines

Summary The condensed bridged isoxazolines4 are rearranged on irradiation with a low-pressure mercury lamp exclusively into condensed derivatives of tetrahydropyridine5. The selectivity of the rearrangement is due to a stabilization of the biradical8 by the overlap of the radical-electrons with -electrons of the C=C double bond and the heterocyclic ring. Quantum yields of the photorearrangement, established from the consumption of the starting materials4, were determined.

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Photochemie kondensierter Isoxazoline

Zusammenfassung Die kondensierten überbrückten Isoxazoline4 werden durch Bestrahlen mit einer Niederdruckquecksilberlampe ausschließlich zu kondensierten Tetrahydropyridinderivaten (5) umgelagert. Die Selektivität der Umlagerung beruht auf der Stabilisierung des Diradikals8 durch Überlappung der ungepaarten Elektronen mit -Elektronen der C=C-Doppelbindung und des Heterocyclus. Aus dem Verbrauch an Ausgangsmaterial (4) wurden Quantenausbeuten der Photoumlagerung bestimmt.

     

Catalytically Active Hollow Fiber Membranes with Enzyme-Embedded Metal–Organic Framework Coating

Metal–organic frameworks (MOFs) are suitable enzyme immobilization matrices. Reported here is the in situ biomineralization of glucose oxidase (GOD) into MOF crystals (ZIF-8) by interfacial crystallization. This method is effective for the selective coating of porous polyethersulfone microfiltration hollow fibers on the shell side in a straightforward one-step process. MOF layers with a thickness of 8 μm were synthesized, and fluorescence microscopy and a colorimetric protein assay revealed the successful inclusion of GOD into the ZIF-8 layer with an enzyme concentration of 29±3 μg cm⁻². Enzymatic activity tests revealed that 50 % of the enzyme activity is preserved. Continuous enzymatic reactions, by the permeation of β-d -glucose through the GOD@ZIF-8 membranes, showed a 50 % increased activity compared to batch experiments, emphasizing the importance of the convective transport of educts and products to and from the enzymatic active centers.     

Rare-earth Metal Borosilicides R9Si15–xB3 (R = Tb,Yb): New Ordered Structures Derived from the AlB2 Structure Type

Two novel ternary borosilicides R₉Si_15–xB₃ (R = Tb, x = 1.80, R = Yb, x = 1.17) were synthesized from the initial elements using tin flux method. Their crystal structures were determined by means of X-ray single crystal diffraction. Both refer to space group R32, Z = 1: a = 6.668(2) Å, c = 12.405(4) Å [R₁ = 0.027, wR₂ = 0.031 for 1832 reflections with I_o > 2σ (I_o)] for Tb₉Si_15–xB₃, and a = 6.5796(3) Å, c = 12.2599(5) Å [R_F = 0.052, wR = 0.090 for 1369 reflections with I_o > 2σ (I_o)] for Yb₉Si_15–xB₃. The structures represent a new structure type, derived from that of AlB₂, with ordering in the metalloid sublattice resulting in distorted [Si₅B] hexagons. The presence or absence of boron in this ordered structure is discussed on the basis of difference Fourier syntheses, interatomic distances, structural analysis, and theoretical calculations in relation with the parent structures of the binaries AlB₂ and Yb₃Si₅ (Th₃Pd₅ type of structure). Theoretical calculations show substantial covalent interactions between the metal and nonmetal elements. The small percentage of silicon atoms, which are missing in these nonstoichiometric compounds, probably allows strengthening boron-metal and boron-silicon bonding.     

The development of microparticulate cellulose-based packing materials and evaluation of potential use in capillary electrochromatography

Summary Expanding the range of stationary phases employed in capillary electrochromatography, the development of rigid cellulose-based micro-beads, their physical-chemical modification and their use in capillary electrochromatography are described. Cellulose-based stationary phases have been employed in the normal-phase and the reversed-phase modes. Presented at the 21^st ISC held in Stuttgart, Germany, 15^th–20^th September, 1996