Bestimmung des Oxydationszustandes in Vanadiumkomplexen mit Hilfe von V—K-Röntgenabsorptionsspektren

Determination of the Oxydation State in Vanadium Complexes using V—K-Absorption Spectra The compounds resulting from the reaction of oxovanadium(IV) sulfate with 8-quinolinols in air were characterized by magnetic moments and V—K-absorption spectra. 8-quinolinol and its Mannich derivates (“CMAB-oxine”, “CMAP-oxine”) form vanadium(V) complexes. The oxovanadium(IV) compound of 7-methyl-8-quinolinol initially formed is not very stable in solution and tends to oxydation. Only the oxovanadium(IV) complex of 2-methyl-8-quinolinol has a good stability corresponding to that of β-diketone compounds.     

Adsorption of neodymium ions on activated charcoal from aqeous solutions

Summary A commercial activated charcoal has been tested as an adsorbent for the removal of neodymium ions from aqueous solutions. The adsorption behavior of neodymium ions on activated charcoal from aqueous solutions has been studied as a function of shaking time, neodymium ions concentration and concentration of different acids. Results reveal that the adsorption equilibrium is attained within 30 minutes, and diffusion of neodymium ions into the pores of activated charcoal controls the adsorption process. The adsorption process follows the first order kinetics. The Langmuir isotherm equation was obeyed well in the whole range of concentration studied. The influence of different cations and anions on the adsorption of neodymium ion from aqueous solutions have also been investigated. Approximately 98% of neodymium ions adsorbed onto activated charcoal could be recovered with 40 ml of 3M HNO₃ solutions.     

Free radicals in electrochemical reduction of 3,5-dicarbethoxy-1,4-dihydropyridines with nitrophenyl groups in positions 2, 4, and 6

In the electrochemical reduction of 2,6-bis- and 2,4,6-tris(nitrophenyl) derivatives of 3,5-dicarbethoxy-1,4-dihydropyridine, in the first stage, one of the para-nitrophenyl groups in position 2 or 6 of the heterocycle is reduced. Free radicals have been obtained and identified, the primary species being ion radicals of the nitrophenyl type. The presence of the heterocycle in the molecule of the 1,4-dihydropyridine derivative stabilizes secondary free radicals of the nitrosophenyl type. In the process of electrochemical reduction, no evidence has been found of any intramolecular transfer of electrons or protons from the dihydropyridine part of the molecule to the nitrophenyl groups. Derivatives of 2,6-bis(p-nitrophenyl)-3,5-dicarbethoxy-1,4-dihydropyridine have been synthesized, and the oxidation and methylation of these derivatives have been studied.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 481–487, April, 1991.     

Inclusion of Nonopiate Analgesic Drugs in Cyclodextrins. I. X-Ray Structure of a 1 : 1 β-Cyclodextrin-p-bromoacetanilide Complex

The preparation and X-ray crystal structure of a 1 : 1 complex between -cyclodextrin (-CD) and the analgesic p-bromoacetanilide are reported. Thermogravimetric and UV spectrophotometric analyses of single crystals grown from an aqueous solution containing host and guest in 1 : 1 molar ratio yielded the composition -CD p-bromoacetanilide $ 13.5H2O. Crystals of the complex are triclinic, space group P1, with a = 15.197(3), b = 15.613(2), c = 15.743(4) Å, = 87.16(2), = 98.29(2), = 103.39(1)° and Z = 2 crystallographically independent complex units per unit cell. The -CD molecules form head-to-head dimers which pack in the channel-mode. Each dimer contains two guest molecules whose acetylamino substituents are located at the dimer interface while the bromine atoms protrude from the -CD primary faces. The acetyl residues of both guest molecules were found to be disordered but the X-ray data permitted     

Infrared and Raman spectral interpretations of the ferroelectric phases of NaH3(SeO3)2 and NaD3(SeO3)2

The infrared and Raman spectra of NaH₃(SeO₃)₂ and NaD₃(SeO₃)₂ have been recorded from 24 to 300°K. The interpretation, assignments, and analysis of the spectral studies are presented on the paraelectric α phase (proton disordered), ferroelectric β phase (proton ordered) and ferroelectric γ phase (proton ordered). A discussion of a newly proposed proton-triggered phase transition mechanism and a possible origin of the hydrogen-bonded OH stretching region of KH₂PO₄-type ferroelectrics is given.     

Determination of isotopic composition of lithium by neutron activation analysis; comparison with mass spectrometry

An activation analysis method is described for routine determination of⁶Li-abundances in various lithium compounds on the basis of the reaction sequence⁶Li(n,α)T and¹⁶O(t, n)¹⁸F and the measurement of¹⁸F. Irradiations of diluted equeous solutions of samples containing CrO₃ as internal flux monitor were carried out at a thermal neutron flux density of ϕ≤10¹¹ n·cm⁻²·sec⁻¹. Interferences from variations in neutron self-shielding oxygen concentration and triton range do not exceed 0.5% when using the dilution technique. The results for⁶Li abundances from 3.52 to 7.60% with standard deviations of 1 to 2.5% were confirmed by mass spectrometric measurements.     

Rapid polarographic method for determining arsenic in steel

A simple and sensitive polarographic method for determining arsenic in steel is presented. The steel is dissolved in HNO(3), and arsenic reduced with Na(2)S(2)O(5)-K.I. The polarographic wave is recorded for an electrolyte at pH 3.0 and containing Fe(II), Mn(II). citric and ascorbic acids. Levels of 0.2% and 0.003% As can be determined with a coefficient of variation of +/- 6%.