29Si-NMR-Untersuchungen zur Anionenstruktur von Kristallinen Tetramethylammonium-alumosilicaten und -alumosilicatlösungen

²⁹Si NMR Investigations on the Anion Structure of Crystalline Tetramethylammoniumaluminosilicates and -aluminosilicate Solutions The ²⁹Si NMR spectra of crystalline tetramethylammonium (TMA) aluminosilicates with different Si/Al ratios exhibit up to 4 sharp signals with characteristic chemical shifts which can be assigned to the central Si atom of OSi(OSi)_3?n(OAl)_n building units of double four-ring (DFR) aluminosilicate anions. The number and distributions of the Al atoms in the DFR framework can be derived from the signal intensities in connection with the results of the trimethylsilylation method [1]. A good agreement of the results of both methods has been found. The DFR can exist as monomeric unit or can be connected to polymeric structures by SiOAl bridges, but no information can be obtained about this question by the ²⁹Si NMR spectra. The investigation of the TMA aluminosilicate solutions by ²⁹Si NMR and TMS method [1] show that stable aluminosilicate anions exist in these solutions. The structure of these aluminosilicate anions is different from the structure of the crystalline TMA aluminosilicates obtained from the solutions.     

Dichten und scheinbare Molvolumina wäßriger Lösungen von Calciumnitrat und Calciumchlorid

Densities and Apparent Molal Volumes of Ca(NO₃)₂? CaCl₂ Aqueous Solutions Densities and apparent molal volumes of Ca(NO₃)₂? CaCl₂ aqueous solutions were determined as a function of temperature and concentration. The dependence of apparent molal volumes on the anion composition is discussed.     

Herstellung und Eigenschaften von Aluminiumaquoxid. I. Böhmit aus Aluminiumnitrat und Ammoniakwasser

Preparation and Properties of Aluminium Hydroxide. I. Boehmite from Aluminium Nitrate and Ammonia The physical-chemical properties of mainly boehmite containing aluminium hydroxide are studied which were made by continuous precipitation from aluminium nitrate solution with ammonia liquor using technical raw materials and test conditions being very similar to those applied in production. The influence of the precipitation conditions (pH value, temperature, concentration and residence time in the precipitation solution) on the composition, structure and texture of the precipitation products is investigated and information about their effect on the filtration behaviour are given. In the case of a continuous precipitation it is possible to obtain phase-pure boehmite being relatively well crystallised. The crystallinity and dispersity of the precipitated hydroxide determine their filterability and the cavity structure.     

Zum Anionenaufbau von Tetra-n-butylammoniumsilicaten und ihren wäßrigen Lösungen

On the Anion Constitutions of Tetrabutylammonium Silicates and their Aqueous Solutions The anion distribution of tetra-n-butylammonium-(TBA)-silicate solutions with molar TBA/SiO₂ ratios between 0.6 and 4 and silica concentrations between 0.1 M and 2.2 M has been investigated by trimethylsilylation and ²⁹Si NMR techniques. In contrast to concentrated tetramethylammonium- and tetraethylammonium silicate solutions in TBA silicate solutions a preference of double ring silicate anions does not occur. In TBA silicate solutions a broad distribution of silicate anions consisting of monomeric, oligomeric chain and ring, as well as polymeric silicate anions has been observed. Crystalline TBA silicates with TBA/SiO₂ ratios of 0.78 to 1 contain mainly double five-ring silicate anions Si₁₀O₂₅^10? whereas for TBA/SiO₂ ratios higher than 1.4 the double three-ring anion Si₆O₁₅^6? predominates. A recently prepared TBA silicate with low TBA content (TBA/SiO₂ = 0.23) has been found to consist of double four-ring silicate anions with 6 SiOH groups per double four-ring.     

Herstellung und Quantifizierung von Polychlordibenzodioxin-Standards

Zusammenfassung Die Herstellung sämtlicher PCDDs (Tetra- bis Octa-) im Mikromaßstab wird beschrieben. Die Identifizierung der Substanzen sowie Möglichkeiten zur Quantifizierung mit dem chlorspezifischen Electrolytic-Conductivity-Detector werden aufgezeigt. Es folgen einige praxisbezogene Hinweise bezüglich der Sicherheitsrichtlinien bei der Herstellung der Standards und Untersuchung von Umweltproben.

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Synthesis and quantification of polychlorodibenzodioxin standards

Summary The micro-scale preparation is described of all the PCDDs (tetra- to octa-), together with the identification of the substances and the feasibility of their quantification by means of the chlorine-specific electrolyte conductivity detector. Some remarks are given concerning safety considerations during the synthesis of the standards and the investigation of environmental samples.

     

Über den Einfluß von Temperatur und Fremdionen auf Eigenschaften und Bau der Natriumwasserglaslösungen

The Influence of Temperature and Impurities Addition on the Properties and the Constitution of Sodium Water Glass Solutions Sodium water glass (NaWG-)solutions of constant composition (SiO₂/Na₂O = 3,3; C_SiO2 = 6,2 M) and different concentration of impurities (Fe, Al, Ti, Cu, chloride, sulfate) were investigated in dependence on temperature by means of the dye absorption method, ¹H- and ²³Na-NMR spectroscopy. It is shown, that the differences in the dye absorption spectra of normalized technical NaWG-solutions, mainly depend on the Fe-concentration in the solutions and their thermal history. From the results follow a crosslinking of polymeric silicate species by Fe? O? Si bonds and/or hydrogen bridges and a fully or partially degradation of these bonds at higher temperatures (150°C).