Ground state correlation energy of the Be-sequence forZ=4–20 in MCDF approximation

The ground state (J=0) electronic correlation energy of the 4-electron Be-sequence is calculated in the Multi-Configuration Dirac-Fock approximation forZ=4–20. The 4 electrons were distributed over the configurations arising from the 1s, 2s, 2p, 3s, 3p and 3d orbitals. Theoretical values obtained here are in good agreement with experimental correlation energies.     

Detection and assessment of citrus tristeza virus antigens by computer-aided scanning densitometry

Citrus tristeza virus (CTV) extracted from Etrog citron (C.medica L.) was immunoprecipitated. The immunoprecipitate was fractionated by SDS-PAGE and western blotted onto nitrocellulose. The CTV antigens were determined by immunoblot analysis using rabbit anti-CTV IgG, and the protein-band pattern exhibited on the nitrocellulose was assessed by soft-laser scanning densitometry. The densitometric tracing revealed the presence of bands that were not visible to the naked eye. Using the superimposition mode of the instrument, it was also revealed that the protein-band patterns of different CTV samples were not identical. Computer-aided soft-laser scanning densitometry proved to be a powerful approach in the detection and assessment of protein bands revealed on nitrocellulose immunoblots, which we were previously unable to do employing conventional methods.     

Spectrophotometric determination ofo- andp-phenylenediamines

Summary Cupric chloride-triphenylphosphine complex gives red color witho-phenylenediamine having maximum absorption at 505–520 nm and 0.5g/ml as visual limit of identification. The reaction is specific foro-phenylenediamine and obeys Beer's law (1 to 10g/ml). This reaction provides the basis of a new method for the Spectrophotometric determination ofo-phenylenediamine ing quantities.Ruthenium trichloride-triphenylphosphine complex gives blue color withp-phenylenediamine having maximum absorption at 580 nm and 2g/ml as visual limit of identification. On the basis of this color reaction a Spectrophotometric method for the determination ofp-phenylenediamine in hair dyes is described. The recovery of the dye from commercial preparations is better than 97%. Other organic compounds do not interfere.

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Zusammenfassung Kupfer(II)chlorid-triphenylphosphin reagiert mito-Phenylendiamin unter Rotfärbung mit maximaler Absorption bei 505 bis 520 nm und 0,5g/ml als Erfassungsgrenze. Die Reaktion ist für o-Phenylendiamin spezifisch und folgt dem Beerschen Gesetz zwischen 1 und 10g/ml. Sie dient als Grundlage für eine neue Methode der spektrophotometrischen Bestimmung von Mikrogrammengen o-Phenylendiamin.Rutheniumtrichlorid-triphenylphosphin reagiert mit p-Phenylendiamin unter Blaufärbung mit maximaler Absorption bei 580 nm und 2g/ml als Erfassungsgrenze. Auf dieser Grundlage läßt sich p-Phenylendiamin in Haarfärbemitteln bestimmen. In handelsüblichen Präparaten werden mehr als 97% des enthaltenen Farbstoffes gefunden. Andere Verbindungen stören nicht.

     

4,4-Acetalidine-bis-(3-methyl isoxazolone-5) as a new colorimetric reagent for the determination of palladium and uranium

Summary Palladium and uranium react with 4,4-acetalidine-bis-(3-methyl isoxazolone-5) in acid medium to give yellow color having a visual limit of identification at 2 and 15g per ml. This color reaction provides the basis of a new method for colorimetric determination of palladium and uranium. Copper also gives yellow color but it cannot be determined with this color reaction because the color intensity is not stable. The maximum tolerable limit of various ions is reported.

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Zusammenfassung Pd und U reagieren in saurem Milieu mit 4,4-Acetalidin-bis-(3-methyl-isoxazolon-5) unter Gelbfärbung mit einer Erfassungsgrenze von 2 bzw. 15g/ml. Diese Farbreaktion dient als Grundlage für eine neue kolorimetrische Methode für Pd und U. Cu gibt zwar auch eine Gelbfärbung, kann aber damit nicht bestimmt werden, da die Farbintensität nicht beständig ist. Die maximal tolerierbare Menge der Fremdionen wird angegeben.

     

Application of high-field NMR and cryogenic probe technologies in the structural elucidation of poecillastrin a,a new antitumor macrolide lactam from the sponge poecillastra species

Poecillastrin A (1), a new polyketide-derived macrolide lactam, was isolated from a deep-water collection of the marine sponge Poecillastra species. The structure of poecillastrin A (1) was assigned using NMR data acquired at 500 MHz with an inverse-detection cryogenic probe and at 800 MHz with a room-temperature probe.     

Equilibrium interaction of solid surfaces across a polymer melt

Forces across polymer melts are poorly understood despite their importance for adhesion and fabricating composite materials. Using an atomic force microscope (AFM), this interaction was measured for poly(dimethyl siloxane) (PDMS). The structure of the polymer at the surface changed during the first approximately 10 h. Afterward, short-range attractive forces were observed with short-chain PDMS (M(w) = 4200 g/mol). Using PDMS with a molecular weight (M(w) = 18 000 g/mol) above the entanglement limit, we measured a monotonically decaying repulsive force, which indicates that a quasi-immobilized layer had formed at the solid surface. Due to the small radius of curvature of the tip, forces could be measured in equilibrium.     

Reductive activation of nitrate reductases

Protein film voltammetry of Paracoccus pantotrophus respiratory nitrate reductase (NarGH) and Synechococcus elongatus assimilatory nitrate reductase (NarB) shows that reductive activation of these enzymes may be required before steady state catalysis is observed. For NarGH complementary spectroscopic studies suggest a structural context for the activation. Catalytic protein film voltammetry at a range of temperatures has allowed quantitation of the activation energies for nitrate reduction. For NarGH with an operating potential of ca. 0.05 V the activation energy of ca. 35 kJ mol-1 is over twice that measured for NarB whose operating potential is ca. -0.35 V.     

Resolving the copper interference effect on the stripping chronopotentiometric response of lead(II) obtained at bismuth film screen-printed electrode

As copper(II) is a common ion in a variety of analytical samples, its effect on the stripping response of lead(II) at bismuth film screen-printed carbon electrode (BFSPCE) was investigated. The study was conducted using a screen-printed three-electrode system (working, counter and reference electrodes), with the carbon-working electrode plated in situ with bismuth film. Copper present at significant concentration level in samples was found to affect the sensitivity of the electrode by reducing the constant current stripping chronopotentiometric (CCSCP) response of lead(II). Recovery of the lead stripping response at the BFSPCE in the presence of copper was obtained when 0.1 mM ferricyanide was added to the test solution. The ferricyanide added circumvents the detrimental effect of copper(II) by selectively masking the copper ions by forming a complex. The analytical utility of the procedure is illustrated by the stripping chronopotentiometric determinations of lead(II) in soil extracts.     

Novel products from attempted michael addition to 1-methyl-1,2,5,6-tetrahydropyridine-4-carbonitrile

The reaction of some phenols with the title compound, in the presence of sodium, gives 2-(2-hydroxyaryl_piperidine derivatives. Geometrical isomers have been separated, which differ in having an equatorial (A) or axial (B) cyano group on the piperidine chair (the methyl and aryl groups are equatorial in both forms). The x-ray crystallographic structures of an example of each of A and B are reported and the proton NMR spectra are assigned.     

Complexes of tris(o-phenanthroline)nickel(II) and copper(II) bromide with dithiocarbamates derived from α-amino acids

Complexes of 1,10-o-phenanthroline (o-phen)-Ni^II and Cu^II with dithiocarbamates derived from -amino acids (glycine, phenylalanine, alanine, methionine and tryptophan) were synthesized and characterized by chemical analysis, spectral and thermal studies and by biological screening; the complexes are non-electrolytes. The empirical formula are [Ni(o-phen)₂(aadtc)] and [Cu₂(o-phen)₂(phaladtc)(H₂O)₂Br₂] where, aadtc = glycinyl-, phenylalaninyl-, alaninyl-, methioninyl- and tryptophanyldithiocarbamate and phaladtc = phenylalaninyldithiocarbamate. The structure of these complexes is probably octahedral. Molecular association through hydrogen bonding between the —NH and the carboxylate groups is proposed for the Ni^II complexes. The Cu^II complex is dimeric with the phenylalaninyldithiocarbamate acting as a bridge.