Die Trennung des Molybd?ns von Yanadium durch Anionenaustauscher als Thioglykolatkomplex und die photometrische Bestimmung des Vanadiums mit Thioglykols?ure

Zusammenfassung Die Trennung der Thioglykolsäurekomplexe des Molybdäns von dem des Vanadiums verläuft mit einer Molybdänausbeute von 99%. Das Vanadium kann im Durchlauf in bequemer Weise mittels Thioglykolsäure im p_H-Bereich 4,5–8 bei guter Genauigkeit photometriert werden.Herrn Prof. Dr. O. Glemser, Direktor des Anorganisch-Chem.-Instituts, danken wir sehr für das stete Interesse und die Unterstützung, die er uns zuteil werden ließ.Dem Herrn Bundesminster für Atomkernenergie und Wasserwirtschaft sowie der Deutschen Forschungsgemeinschaft danken wir für apparative und finanzielle Hilfe.     

Beitrag zur Analyse von Stibin

Zusammenfassung Es wird ein Verfahren zur Bestimmung von Stibin beschrieben, das sich sowohl zur Analyse von SbH₃ in organischen Lösungsmitteln als auch zur Bestimmung von flüssigem oder festem SbH₃ eignet. Hierbei wird das Stibin mit überschüssigem Brom zu Sb^V oxydiert, danach mit SO₂ zu Sb^III reduziert und dieses oxydimetrisch mit Jod oder Bromat titriert.

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Summary A method is proposed for the determination of stibine, applicable to its solutions in organic solvents and also to the solvent-free liquid or solid substance. The procedure involves oxidation of SbH₃ with an excess of bromine to Sb^V, reduction to Sb^III with SO₂, and oxidimetric titration of the trivalent antimony with iodine or bromate.

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Herrn Professor Dr. C. Mahr zum 65. Geburtstag gewidmet.     

Macroscopic mass and energy balance of a pilot plant anaerobic bioreactor operated under thermophilic conditions

Intensive poultry production generates over 100,000 t of litter annually in West Virginia and 9×10⁶ t nationwide. Current available technological alternatives based on thermophilic anaerobic digestion for residuals treatment are diverse. A modification of the typical continuous stirred tank reactor is a promising process being relatively stable and owing to its capability to manage considerable amounts of residuals at low operational cost. A 40-m³ pilot plant digester was used for performance evaluation considering energy input and methane production. Results suggest some changes to the pilot plant configuration are necessary to reduce power consumption although maximizing biodigester performance.     

Photofragmentation of dichloromethanol Cl2CHOH along C-O and C-Cl cleavages: a theoretical study

Multireference configuration interaction calculations are carried out for ground and excited states of dichloromethanol, Cl2CHOH, to investigate two important photofragmentation processes relevant to atmospheric chemistry. Five low-lying excited states (1(1)A", 2(1)A', 1(3)A", 2(3)A" and 1(3)A') in the energy range between 6.4 and 7.5 eV are found to be highly repulsive for C-Cl elongation, leading to ClCHOH (X2A) and Cl (X2P). Photodissociation along the C-O bond resulting in CHCl2 (X2A') and OH (X2II) has to overcome a barrier of about 0.5 eV because the low-lying excited states 1(1)A", 1(3)A' and 1(3)A" become repulsive only after the C-O bond is elongated by about 0.3 A.     

Cyclopeptid-Antibiotika aus Aspergillus-Arten. Struktur der Echinocandine C und D

Cyclopeptide antibiotics from Aspergillus species. Structure of echinocandins C and D The echinocandins B, C and D are antifungal antibiotics produced by a strain of Aspergillus rugulosus. All three metabolites are closely related representing cyclic oligopeptides composed of six amino acids and a linolic acid residue in an amide linkage. The complete structure of echinocandin B ( 1 ) has recently been established by X-ray analysis. Structural assignments to the new minor metabolites C and D have now been made by hydrolytic and oxidative cleavage reactions, formation of N-acyl-α-aminoethers as well as by chemical correlations and extensive NMR. examinations. Echinocandin C ( 2 ), C₅₂H₈₁N₇O₁₅, contains 3-hydroxyhomotyrosine in the place of 3, 4-dihydroxyhomotyrosine present in 1 . Echinocandin D ( 3 ), C₅₂H₈₁N₇O₁₃, differs in two amino acids: 3, 4-dihyroxyhomotyrosine and 4, 5-dihydroxyornithine, unusual units of 1 being replaced by 3-hydroxyhomotyrosine and ornithine.     

A versatile synthesis of new pyrimidinyl nitronyl nitroxides

Pyrimidinyl nitronyl nitroxides where the bis-N-oxy fragment is included in a six-membered ring were prepared from diacetonamine by a sequence of reactions including a Grignard reaction, a Ritter reaction and oxidation of the intermediate pyrimidine; the properties of the 2-phenyl-substituted representative are fully described.     

Stoffwechselprodukte von Mikroorganismen. 211. Milteilung. Röntgenstrukturanalyse von Elaiophylin

The X-ray crystal structure analysis of the antibiotic elaiophylin ( 1 ), monoclinic, a = 9.927, b = 10.105, c = 31.183 Å, β = 93.20°, space group P2₁, confirms the constitution elucidated by spectroscopic methods and chemical degradation. In the crystal the two chemically equivalent halves of the molecule are related by an approximate twofold rotation axis.     

ITQ-15: the first ultralarge pore zeolite with a bi-directional pore system formed by intersecting 14- and 12-ring channels, and its catalytic implications

The pore topology of ITQ-15 zeolite consists of an ultra-large 14-ring channel that is intersected perpendicularly by a 12-ring pore; acid sites have been introduced in its framework and this unique structure shows advantages over unidirectional ultralarge pore zeolites for diffusing and reacting large molecules.     

Time-resolved investigations of singlet oxygen luminescence in water, in phosphatidylcholine, and in aqueous suspensions of phosphatidylcholine or HT29 cells

Singlet oxygen was generated by energy transfer from the photoexcited sensitizer, Photofrin or 9-acetoxy-2,7,12,17-tetrakis-(beta-methoxyethyl)-porphycene (ATMPn), to molecular oxygen. Singlet oxygen was detected time-resolved by its luminescence at 1270 nm in an environment of increasing complexity, water (H2O), pure phosphatidylcholine, phosphatidylcholine in water (lipid suspensions), and aqueous suspensions of living cells. In the case of the lipid suspensions, the sensitizers accumulated in the lipids, whereas the localizations in the cells are the membranes containing phosphatidylcholine. By use of Photofrin, the measured luminescence decay times of singlet oxygen were 3.5 +/- 0.5 micros in water, 14 +/- 2 micros in lipid, 9 +/- 2 micros in aqueous suspensions of lipid droplets, and 10 +/- 3 micros in aqueous suspensions of human colonic cancer cells (HT29). The decay time in cell suspensions was much longer than in water and was comparable to the value in suspensions of phosphatidylcholine. That luminescence signal might be attributed to singlet oxygen decaying in the lipid areas of cellular membranes. The measured luminescence decay times of singlet oxygen excited by ATMPn in pure lipid and lipid suspensions were the same within the experimental error as for Photofrin. In contrast to experiments with Photofrin, the decay time in aqueous suspension of HT29 cells was 6 +/- 2 micros when using ATMPn.     

Nouveaux heterocycles tricycliques synthese de derives de l'aza-2 pyrrolo[1,2-a]indole

The synthesis of aza-2 pyrrolo[1,2-a]indole derivatives was achieved by a 1,3-dipolar cycloaddition reaction of dimethylacetylenedicarboxylate with a mesoionic ion.