Cyano-bridged CuII-MV (M = Mo, W) bimetallic layered complexes exhibiting novel honeycomblike structures

Self-assembly of a new precursor [Cu(L)](ClO4)2 (1) (L = macrocyclic ligand) with octacyanometalates [M(CN)8]3- (M = Mo, W) produced two-dimensional cyano-bridged Cu(II)-M(V) bimetallic assemblies [Cu(L)]3n[M(CN)8]2n.6nH2O [M = Mo (2), W (3)] with novel honeycomblike structures, characterized by spectroscopic data, single-crystal X-ray diffraction studies, and magnetic measurements. The crystallographic determination reveals that compounds 2 and 3 are isostructural and crystallize in the triclinic system (P). The Cu atom in a distorted octahedral environment experiences a tetragonal elongation of apical nitrogen atoms exhibiting average Cu-Nax lengths of 2.566 Angstroms for 2 and 2.593 Angstroms for 3, which accounts for the Jahn-Teller effect of a Cu(II) ion. The Cu-NC angles are magnetically important, ranging from 135.7 to 159.2 degrees. Three types of L in the crystal lattice are observed, which are dependent on the relative positions of the pendant hydroxyl groups with respect to the CuN4 basal plane. The positions are correlated with hydrogen bonding of OH groups to neighboring atoms. The magnetic data indicate that ferromagnetic and antiferromagnetic interactions between Cu(II) and M(V) through the CN linkage coexist.     

Gas chromatographic determination of estrone,estradiol and estriol in non-pregnancy plasma

Summary A gas Chromatographic method for the determination of estrone, estradiol and estriol in plasma of normal females is described. Purification is done by means of TLC of the free compounds and the acetates and quantitation is achieved by electron capture-gas chromatography of the estrogen heptafluorobutyrates. Experiments on the validation of the method are described along with some examples of its application.

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Zusammenfassung Eine gaschromatographische Methode zur Bestimmung von Östron, Östradiol und Östriol im normalen weiblichen Plasma wurde beschrieben. Die Reinigung erfolgte durch Dünnschichtchromatographie der freien Verbindungen und ihrer Acetate. Die quantitative Bestimmung wurde gaschromatographisch mit Hilfe eines Elektroneneinfangdetektors an Hand der Östrogenheptafluorobutyrate bewerkstelligt. Versuche zur Bewertung dieser Methode sowie Beispiele für ihre Anwendung wurden beschrieben.

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Supported by USPHS Grants AM 09908 and RCDA 5 K 3-AM-31, 321 (S. K.) and a grant from the Ford Foundation.     

Pore size distributions in low‐k dielectric thin films from X‐ray porosimetry

X‐ray reflectivity has been used to determine the mass uptake of probe molecules in porous thin films supported on thick silicon wafers. The adsorption occurs by capillary condensation when the films are exposed to probe vapor at controlled partial vapor pressures. The probe solvent partial pressure was varied by mixing saturated air and dry air at constant temperature or by changing sample temperature at a constant vapor concentration. Pore size distribution in the films can be calculated from the probe uptake with typical porosimetric approaches such as the application of the Kelvin equation to convert partial pressure into pore size. For illustration, the pore size distribution of three different nanoporous thin films, the primary candidate of ultra‐low‐k interlevel dielectrics in the next generation of integrated circuit chips, was determined with this technique. These samples represent different generations of low‐k dielectrics developed by industry. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 40: 2170–2177, 2002     

Studies on mass production of transformed Panax ginseng hairy roots in bioreactor

The growth properties of Panax ginseng hairy roots transformed by Agrobacterium rhizogenes were compared between flask and aerated column or stirred bioreactor. In flask cultures, sucrose, initially 30 g/L, was nearly exhausted after 45 d of culture. The pH of the medium dropped from 5.5 to 4.96 after 10 d, but afterward it gradually increased to 6.4. After 45 d, hairy roots grew about 16-folds. The growth rate of hairy roots in air-bubble column or stirred bioreactor cultures was 1.13 (1.11) to 1.23 (1.20) g fresh wt (dry wt)/(g of cells·d), respectively. For both bioreactors, growth was about three times as high as in the flask cultivation.     

Polyarylate–polystyrene block copolymer from macro-azoinitiator: Synthesis and its thermal properties

A macro-azoinitiator containing polyarylate segment and azo group was prepared by the solution polycondensation of azobiscyanopentanoyl chloride and hydroxy-terminated polyarylates having viscosity-average molecular weights of 6200, 8100, and 12 400. These macro-azoinitiators were used in the radical polymerization of styrene to synthesize polyarylate-polystyrene block copolymers. Thermal properties measured by the differential scanning calorimetry indicated the phase separated morphology of the block copolymers except at low molecular weight of the block constituents. © 1993 John Wiley & Sons, Inc.