Zusammenhang von elektrochemischkonstitutivem und kolloidem Aufbau reinster Farbsole

Zusammenfassung 1. Es werden mittels Elektrodialyse und Elektrodekantierung die hochgereinigten azidoiden blauen Farbsole aus Congorot, Congorubin, Congokorinth G, Benzopurpurin 4 B und Chicagoblau 6 B sowie zum Vergleich das basische Farbsol von Nachtblau hergestellt. 2. Diese Sole werden in bezug auf ihre elektrochemischkonstitutiven sowie Assoziations?nderungen durch Bestimmung ihrer thermischen Leitf?higkeitsabh?ngigkeit (x, t-Kurve) und deren Reversibilit?t sowie der Verdünnungs?nderung ihrer molekularen Leitf?higkeiten μ untersucht. 3. Es wird gezeigt, wie bei den genannten azidoiden Farbsolen, die s?mtliche Aminosulfos?uren darstellen, die Assoziationskr?fte mit der inneren Salzbildung wachsen und wie andererseits mit der Zunahme der polaren sauren Gruppen infolge der thermischen oder Verdünnungsaminolyse des inneren Salzes die Desassoziation erh?ht wird. Das Nachhinken der Leitf?higkeitswerte beim Wiederabkühlen ist der Ausdruck einer Assoziationshysteresis. Mit der Zeit stellt sich beim Stehen ein Assoziationsgleichgewicht ein. 4. Gegenüber dem Congoblau weisen Congorubin und Congokorinth eine Verminderung um eine NH₂-Gruppe, dagegen eine zus?tzliche OH-Gruppe auf, welche je nach ihrer Stellung den sauren Charakter mehr oder weniger verst?rkt. Die Halbierung der inneren Salzbildung und die Steigerung der Gesamtladung pr?gen sich genau in der zu erwartenden Reihenfolge steigender molekularer Leitf?higkeit und der Desassoziation aus. Auch das Verhalten des azidoiden Benzopurpurin- und Chicagoblausols ist hinsichtlich desx, t-Ganges und der μ-Werte sowie der Kolloid?quivalente durchaus das konstitutiv erwartete. 5. Es lassen sich plausible Modelle des Aufbaues der verschiedenen ionischen Micellen bei den einzelnen Farbsolen aufstellen. 6. Die Beziehungen der Farbsole zu den Seifensolen einerseits und den Proteinsolen andererseits werden kurz er?rtert.     

Absorptionsflammenspektrometrische Analysen mit Mikroliter-Proben

Zusammenfassung Es wird beschrieben, wie man unter Verwendung einer Zerstäuber-Brenner-Kombination und eines Lichtstrahloscillographen die benötigte Probenmenge für flammenphotometrische Emissions-oder Absorptions-analysen drastisch senken kann, um eine vorherige Anreicherung des Analysengutes bei kleinen Probenmengen zu ermöglichen. Dazu werden im einzelnen die Meßergebnisse mitgeteilt bezüglich der relativen Schwan-kung des Photostromes, der Einstellzeit der quasistationären Atom-konzentration in der Flamme, der benötigten Probenmenge pro Analyse und die erreichten relativen und absoluten unteren Nachweisgrenzen.

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Summary A method is given by which a preliminary enrichment of the analytically essential material is accomplished so that the amount of sample needed for a flame-photometric determination may be drastically reduced. This is accomplished by using an atomizer-burner combination and a light ray oscillograph. The data regarding the relative fluctuation of the photoflame, the weight of the sample required per analysis and the relative and absolute lower detection limits reached are given in detail.

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Résumé On décrit l'emploi d'un système pulvériseur-brûleur et d'un oscillographe permettant de diminuer considérablement la quantité de prise d'essai nécessaire pour les analyses par photométrie de flamme en émission ou en absorption, ce qui rend possible l'enrichissement préable du produit à analyser dans le cas de petites prises d'essai. On communique en détail les résultats d'analyse concernant la variation relative du courant photoélectrique, la durée d'établissement de la concentration atomique quasi-stationnaire dans la flamme, la prise d'essai nécessaire par analyse et les limites de dilution inférieures atteintes en valeur absolue et en valeur relative.

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Unterstützt mit Mitteln der Deutschen Forschungsgemeinschaft.     

Modulating dopant segregation in floating-zone silicon growth in magnetic fields using rotation

The feasibility of modulating dopant segregation using rotation for floating-zone silicon growth in axisymmetric magnetic fields is investigated through computer simulation. In the model, heat and mass transfer, fluid flow, magnetic fields, melt/solid interfaces, and the free surface are solved globally by a robust finte-volume/Newton's method. Different rotation modes, single- and counter-rotations, are applied to the growth under both axial and cusp magnetic fields. Under the magnetic fields, it is observed that dopant mixing is poor in the quiescent core region of the molten zone, and the weak convection there is responsible for the segregation. Under an axial magnetic field, moderate counter-rotation or crystal rotation improves dopant uniformity. However, excess counter-rotation or feed rotation alone results in more complicated flow structures, and thus induces larger radial segregation. For the cusp fields, rotation can enhance more easily the dopant mixing in the core melt and thus improve dopant uniformity.     

Oriented polycrystalline α-HgI2 thick films grown by physical vapor deposition

This work investigates the growth of polycrystalline α-HgI₂ thick films from physical vapor deposition. By varying the growth conditions, the as-deposited thick films are characterized by scanning electron microscopy, X-ray diffraction, current–voltage and photoconductivity measurements. The growth mechanism and its effects to the properties of these polycrystalline α-HgI₂ thick films are then discussed. Finally, the best deposition conditions for polycrystalline α-HgI₂ thick films compactly formed by separated columnar monocrystallines with uniform orientation along c-direction and with good crystallinity are reported.     

Crystal Structure and Hirshfeld Surface Analysis of Bis(3-thienoyl) Disulfide

The spectroscopic characterization (¹H, ¹³C{¹H} NMR, UV–Vis) and single-crystal X-ray diffraction (scXRD) analysis accomplished by inspection of the Hirshfeld surface of bis(3-thienoyl) disulfide (1) is described. The title compound 1 crystallizes in the monoclinic space group P2₁/n. The unit cell parameters are a?=?7.9959(3) Å, b?=?6.4348(3) Å, c?=?22.4924(9) Å, β?=?100.108(4)°, V?=?1139.32(8) ų, Z?=?4, R_gt(F)?=?0.0278, wR_ref(F²)?=?0.0667. The packing of 1 is dominated by S?O and S?S interactions, giving a 2D layer structure parallel to (101). The X‐ray crystal structure analysis revealed the packing of 1 is dominated by S?O and S?S interactions, giving a 2D layer structure parallel to (101). The intermolecular interactions in 1 were analyzed using the Hirshfeld surface method including 2D fingerprint plots and enrichment ratios (E), which shows that the most favored intermolecular contacts are the O?H and C?S indicated by E values above 1.30. The interaction energies between molecular pairs revealed the importance of the weak O?H and C?S interactions in stabilizing the molecular structure of 1.

Graphic Abstract

Single crystal X-ray structure analysis, DFT calculations and Hirshfeld surface analysis to identify intermolecular interactions within the solid state structure of bis(3-thienoyl) disulfide (1).

     

Synthesis, thermal and magnetic properties of new metal iodate: (LiFe1/3)(IO3)2

This paper reports the detail synthesis of a new kind of metal iodate, anhydrous (LiFe_1/3)(IO₃)₂, from aqueous solutions. The synthesized compound shows spinal morphology and is chemical stable up to 400°C. The iodate shows paramagnetic behavior from room temperature down to 4.2 K. At room temperature, the new compound has a hexagonal structure with the lattice parameters a=5.4632(2) Å, c=5.0895(6) Å, Z=1, space group of P6₃.     

Parallel-oriented fibrogenesis of a beta-sheet forming peptide on supported lipid bilayers

Peptide self-assembly on substrates is currently an intensively studied topic that provides a promising strategy for fabrication of soft materials and is also important for revealing the surface chemistry of amyloidogenic proteins that aggregate on cell membranes. We investigated the fibrogenesis of a beta-sheet forming peptide Abeta(26-35) on supported lipid bilayers (SLBs) by in situ atomic force microscopy (AFM), circular dichroism (CD), and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy. The results show that the Abeta(26-35) nanofilaments' growth is oriented to a specific direction and formed a highly ordered, large-scale, parallel-oriented surface pattern on membranes. The parallel-oriented fibrogenesis of Abeta(26-35) was able to occur on different lipid membranes rather than on solid substrates. It implies that the parallel-oriented fibrogenesis was associated with the distinct properties of lipid membranes, such as the fluid nature of lipid molecules on membranes. The membrane fluidity may allow the peptide assemblies to float at the water-membrane interface and easily orient to an energetically favorable state. These results provide an insight into the surface chemistry of peptide self-assembly on lipid membranes and highlight a possible way to fabricate supramolecular architectures on the surface of soft materials.     

Determination of estrogens in wastewater using three-phase hollow fiber-mediated liquid-phase microextraction followed by HPLC

Three-phase hollow fiber-mediated liquid-phase microextraction followed by HPLC was used for the determination of three synthetic estrogens, namely diethylstilbestrol, dienestrol, and hexestrol, in wastewater. Extraction conditions including organic solvent, volume ratio between donor solution and acceptor phase, extraction time, stirring rate, donor phase and acceptor phase were optimized. The target compounds were extracted from a 10 mL aqueous sample at pH 1.5 (donor solution) through a 45 mm in length hollow polypropylene fiber that was immersed in 1-octanol in advance, and then the hollow fiber was filled with 10 microL 0.5 mol/L sodium hydroxide solution (acceptor phase). After a 40 min extraction, the acceptor phase was directly injected into an HPLC system for detection. Under the optimized extraction conditions, a large enrichment factor (more than 300-fold) was achieved for the three estrogens. The determination limit at an S/N of 3 ranged from 0.25 to 0.5 microg/L for the estrogens. The recovery ratio was more than 86% in the determination of these estrogens in wastewater.     

Hydrothermal synthesis of 2D ordered macroporous ZnO films

The ZnO films with two-dimensional ordered macroporous structure were successfully fabricated through hydrothermal crystal growth of ZnO on the ZnO substrate covered with a monolayer of polystyrene (PS) spheres as template. The precursor solution of hydrothermal crystal growth of ZnO were prepared by equimolar solution of Zn(NO₃)₂·6H₂O and hexamethylenetramine (HMT). The confinement effect of the PS spheres template on the growth of ZnO nanorods and the influence of sodium citrate on the crystal growth of ZnO had been studied. The film surface morphology and the preferential growth of ZnO crystal were investigated by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. Also, the photoluminescence spectrum of ZnO films had been measured, and the corresponding mechanism was discussed. __________ Translated from Chemistry, 2007, 70 (8): 587–592 [译自: 化学通报]