Ionophore vom Typ der 3-Oxapentandiamide

Ionophores of the Type of 3-Oxapentane Diamides A series of lipophilic 3-oxapentane diamides were prepared and their selectivity in membranes was studied. N, N, N′, N′-Tetracyclohexyl-3-oxapentane diamide forms 1:2- and 1:3-metal/ligand-complexes with Mg²⁺ and Ca²⁺ respectively and induces a selectivity in membranes for Ca²⁺ over Mg²⁺ by a factor of about 10⁴.     

Zur Phosphorbestimmung in insecticiden vom Typ der Methyl- und Dimethylphosphon- und -thiophosphons?uren

Ohne Zusammenfassung     

Zur Kenntnis der Chlorid-Spinelle Li2MgCl4, Li2MnCl4, Li2FeCl4, Li2CdCl4

About the Chloride Spinels Li₂MgCl₄, Li₂MnCl₄, Li₂FeCl₄, Li₂CdCl₄ FIR, Raman, and X-ray data of the spinel type chlorides Li₂TCl₄ (T = Mg, Mn, Fe, Cd) are presented. The vibrational spectra indicate that there is no 1:1 ordering on the octahedral sites of the lattice. Both DTA measurements and high temperature X-ray photographs show that the chloride spinels undergo a reversible phase transition to a cubic high temperature defect structure at 535°C (Li₂MgCl₄), 460°C (Li₂MnCl₄) and 385°C (Li₂CdCl₄), which has unit cell dimensions two times smaller than the spinel lattice. Disordering of the lithium sublattice still begins at much lower temperatures, as measurements of the electric conductivity indicate.     

Dealuminierte Molekularsiebe vom Typ Y Zur Porosität dealuminierter Molekularsiebe

Dealuminated Molecular Sieves of Y-Type. To the Porosity of Dealuminated Molecular Sieves The pore volumes and pore size distributions of three dealuminated zeolites are investigated by adsorption and mercury porosimetric measurements. The origin of the secondary pores is discussed.     

Über Oxothallate der Alkalimetalle. Zur Kenntnis von Li5TlO4

New obtained is Li₅TlO₄ (light yellow), which due to single crystal data crystalises with a = 13.23, c = 4.72₈ Å; Z = 8, tetragonal P4₂/nmc. For 342 hk0–hk3, Mo–K_α, is R = R' = 0.098₄ (Parameters see text). Corresponding to Li₅□₂TlO₄, it is an ordered derivative of the Li₂O type of structure.     

Die Verwendung von Klathraten der Komplexsalze vom Typ Ni(SCN)2(4-MePy)4 zur Trennung vonCis-Trans-Azobenzolgemischen

Zusammenfassung Zur Trennung voncis- undtrans-Azobenzol wurden Klathrate des Typs Ni(SCN)₂(4-Methylpyridin)₄·0,7(4-Methylpyridin) erfolgreich als Adsorbentien in chromatographischen Säulen verwendet.Die thermische und photochemischecis-trans-Isomerisierung dieser Verbindungen (bei Zimmertemp.) wurden als mögliche Fehlerquellen bei der quantitativen Auswertung der Trennergebnisse untersucht.

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The application of clathrates formed from complex salts of the Ni(SCN)₂(4-methylpyridine)₄ type to the separation of mixtures of cis- and trans-azobenzenes

The clathrates of Ni(SCN)₂(4-methylpyridine)₄·0,7(4-methylpyridine) type have been successfully applied as sorbents in chromatographic columns to the separation of geometric isomers ofcis- andtrans-azobenzenes.Thermal and photochemicalcis-trans-isomerization of these compounds (at room temperature) have been studied as possible source of errors in the quantitative evaluation of separation results.

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Mit 3 Abbildungen

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Herrn Prof. Dr.H. Nowotny gewidmet.     

Infrarotspektroskopische Untersuchungen der Adsorption von SO2 an Zeolithen vom Typ A

Ohne Zusammenfassung     

Zur Trennung der Thorerde vom Ceroxyd

Ohne Zusammenfassung     

Menge und Zusammensetzung der Carbide in einem niobhaltigen Schnellarbeitsstahl vom Typ M7

Zusammenfassung An einem unkonventionellen Schnellarbeitsstahl vom Typ M7 (2% Wolfram, 9% Molybdän, 1% Vanadin, 1% Niob, 4% Chrom) wurde gezeigt, wie durch gezielte Kombination von Interferenzschichtmetallographie, besonderen rasterelektronenmikroskopischen Abbildungsmethoden, EDX-Analyse und Röntgenbeugungsanalyse eine sichere Identifizierung der Carbidphasen möglich ist. Die Methodenkombination gestattet die Charakterisierung der Carbidphasen und deren Änderung hinsichtlich Menge und chemischer Zusammensetzung in verschiedenen Wärmebehandlungszuständen vom Guß bis zum Härtegefüge.

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Volume fractions and compositions of the carbide phases in a Nb-alloyed M7 high speed steel

Summary Volume fractions were determined by quantitative microscopy from scanning and photoelectron emission micrographs, compositions by EDX analysis in SEM. The identity of the various carbide phases was established by EDX, X-ray diffraction, SEM contrast, and by comparison with color interference microscopy. MC, M₆C and M₂C each occurred in several variants with different compositions and lattice constants; the relation between these phases is discussed against the background of the solidification process of the steel. The metallurgical effect of Nb is to expel most of the V, W and Mo from the MC phase; these elements are accommodated in M₂C and M₆C whose iron content is correspondingly reduced. Only by the combination of the methods mentioned the complete analysis of the carbide phases could be accomplished. The submicroscopic carbides involved in secondary hardening were not part of the study.

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Vortrag für das 10. Kolloquium über metallkundliche Analyse, Wien, 3.–5. November 1980. -Herrn Prof. Dr. Hanns Malissa zum 60. Geburtstag gewidmet.     

Ternäre Bromide und Iodide zweiwertiger Lanthanide und ihre Erdalkali-Analoga vom Typ AMX3 und AM2X5

Ternary Bromides and Iodides of Divalent Lanthanides and Their Alkaline-Earth Analoga of the Type AMX₃ and AM₂X₅ Metallothermic reduction of the tribromides and -iodides MX₃ (M = Sm, Dy, Tm, Yb) with alkali metals as well as with indium and thallium (A = Cs, Rb, K, In, Tl) results in most cases in ternary compounds with the composition AMX₃ and AM₂X₅, respectively. Analogous compounds with M = Ba, Sr, Ca were synthesized from the binary components. The AMX₃ compounds crystallize with the following types of structure: the perovskite-type and its distorted variants, the NaNbO₃-II- and the GdFeO₃-type, the NH₄CdCl₃- and the stuffed PuBr₃-type. These structure types differ by a gain of condensation of the [MX₆] octahedra (three-dimensional connection via corners within the variants of the perovskite-type, double chains of edge- and face-connected octahedra within the NH₄CdCl₃-type, and layers of corner- and edge-connected octahedra within the stuffed PuBr₃-type of structure). This comes along with a reduction of the coordination number of A⁺ from 12 (“ideal” perovskite) to 8 + 2 (GdFeO₃-type), 9 (NH₄CdCl₃-type), and 8 (stuffed PuBr₃-type). Thus, the A/[MX₆] size ratio determines which AMX₃ type of structure is adopted. If the M²⁺ ion is large enough, ternary compounds with the composition AM₂X₅ occur either in addition to the AMX₃ compounds or exclusively. They crystallize with the TlPb₂Cl₅ type of structure (C.N.(M²⁺) = 7 and 8). All of the AMX₃ and AM₂X₅ compounds are summarized in a structure field diagram.     

Zur Kenntnis der Systeme Li2O/CoO und Li2O/ZnO

On the Systems Li₂O/CoO and Li₂O/ZnO According to powder photographs the systems Li₂O/CoO and Li₂O/ZnO are so far similar as the Li-richest phase in near ?Li₄MO₃”?. Single crystal investigations lead to a pseudocubic, trigonal unit cell; a = 13.14, c = 7.99 Å (Zn); a = 13.10, c = 7.98 Å (Co). The oxygen form a cubic closest packing. Surprisingly there is obviously no completely ordered arrangement of cations. In spite of single crystal data the extent of the phases is still unknown.     

Zur Chemie der 4-Aminothiazolin-2-thione

4-Aminothiazolin-2-one-hydrazones3 are obtained by succesive treatment of the title compound1 with dimethyl sulfate and hydrazinehydrate. The rearrangement of 4-aminothiazolin-2-ylidenmalononitrile7 derived from1 yields the 2,4-diamino-thiophene derivatives8. Analogously, the 4-aminothiazolin-2-yliden-cyanamides10 react to form the substituted 2,4-diaminothiazoles11. Succesive reaction of the ethyl (4-amino-2-thioxo-thiazolinyl-3)-acetates12 with dimethyl sulfate and malononitrile yields the 3,6-diamino-pyrrolo[2,1-b]-thiazoles14.

     

Zur Kenntnis der Reaktionsfähigkeit des 5-Methyl-4-ethyl-2-propanonyl-thiazols

The methylene group of 5-methyl-4-ethyl-2-propanonyl-thiazol (II) reacts with different aldehydes yielding theKnoevenagel-condensation products (1–14). The reactions ofII with amines or ammonia gives exclusively the enamines as demonstrated by the¹H-NMR-spectrum (15–23). The reaction product fromII with ammonia (23) can be further transformed to the corresponding derivatives of urea (24–27) with isocyanates.II reacts with acylchlorides in pyridine to the 0-acylation compounds (28–32) and with isocyanates to the corresponding urethanes (38–40).

     

Komplexbildung von Ionophoren vom Typ der Dioxakorksäurediamide mit Alkali- und Erdalkaliionen. Stabilitätskonstanten in Äthanol

Complex Formation of Ionophores of the Dioxaoctane Dicarboxylic Acid Diamide Type with Alkali and Alkaline Earth Cations. Stability Constants in Ethanol. Stability constants are reported for two noncyclic, neutral ionophores in interaction with alkali and alkaline earth metal cations in ethanol. The ligands studied give high selectivity of alkaline earth in respect to alkali metal cations when used in liquid membrane electrodes.     

Zur thermischen Zersetzung vom (NH4)2[FeF5(H2O)] unter quasi-isobaren Bedingungen

On the Thermal Decomposition of (NH₄)₂[FeF₅(H₂O)] on Quasi-Isobaric Conditions The thermal decomposition of (NH₄)₂[FeF₅(H₂O)] was investigated by thermal and X-ray analysis. Quasi-isobaric conditions are realized by using a special crucible which guaranteed a pressure of the gaseous products of 70 kPa. In dependence on the partial pressure α- or β-(NH₄)₂FeF₅ were formed during dehydration. Further intermediate products are NH₄FeF₄, (NH₄)_1?xFeF_4?x, and (NH₄)_yFeF₃ with x = 0.15–0.20 and y = 0.12–0.15. Structural relations between these phases are discussed and comparable considerations to the Al system were made.     

Die Kristallstruktur der Verbindung Li2ZnGeO4

The crystal structure of dilithiumzine orthogermanate, Li₂ZnGeO₄, has been determined and refined byFourier syntheses and least-squares, using three dimensional single-crystal data. A finalR-value of 5.7% was obtained. The monoclinic unit cell (Pn–C_s ²) with the dimensionsa=6.40,b=5.45,c=5.04 Å and =90.2° contains two formula units Li₂ZnGeO₄. The crystal structure is built up by [GeO₄] tetrahedra, which are linked together by [LiO₄] and [ZnO₄] tetrahedra. The average interatomic distances are found to be: Ge–O=1.77, Li–O=2.01 and Zn–O=1.93 Å.