Using radiotracer solutions of Hg (203Hg) and Os (185Os), techniques have been developed for sampling these elements presumably suitable for ion probe measurements. Mercury has been electrodeposited on the cross-sectional area (5 mm2) of an electrochemically pure Cu wire giving a recovery 25 to 30% at the tip. Similar efficiency is found for Hg distillate solutions. Osmium has been collected in a Ni–NiS bead after loading its thiourea complex solution on filter paper. The recovery in the bead is 80–90%. These methods should be of help for isotopic study of these elements by ion microprobe. The suitability of these samples for measurements remains unconfirmed. 相似文献
Diamagnetic susceptibilities of trimethyl(imino-oxy)silanes,Me3SiON CMeR, and dimethyldi(imino-oxy)silanes,Me2Si(ON CMeR)2, containing Si–O bonds are reported. M of these silicon compounds has been calculated theoretically from the method ofBaudet et al. and a good agreement has been obtained between the observed M values and the corresponding calculated values. Si in these compounds has been calculated graphically and the lower values have been explained on the basis of back-bonding to the silicon atom from the oxygen lone pair. 相似文献
A density-functional theory is presented to study the structure of polymers, having attractive interactions, confined between attractive surfaces. The theory treats the ideal-gas free-energy functional exactly and uses weighted density approximation for the hard-chain contribution to the excess free-energy functional. The bulk interactions of freely jointed hard spheres are obtained from generalized Flory equation of state and the attractive interactions are calculated using the direct correlation function obtained from the polymer reference interaction site model theory along with the mean spherical approximation closure. The theoretical predictions are found to be in quite good agreement with the Monte Carlo simulation results for varying densities, chain lengths, and different interaction potentials. The results confirm important implications of using different approximations for the hard-sphere and attractive interactions. 相似文献
A new molybdenum(VI) complex, Li2[Mo2O6(C2O4)] · 2 H2O (LMO), was prepared and characterized by chemical analysis and IR spectral studies. Its thermal decomposition was studied by using TG and DTA techniques. LMO loses its two moles of water between 75 and 170° to give the anhydrous product, which decomposes in three stages between 240 and 380°. The first two stages occur in the temperature ranges 240–280° and 280–305°, to give intermediates with the tentative compositions Li6[Mo6O19(C2O4)2] and Li6[Mo6O20(C2O4)], respectively. In the third stage, which extends up to 380°, Li6[Mo6O20(C2O4)] decomposes to give the end-product, Li2Mo2O7.
Zusammenfassung Ein neuer Molybdän(VI)-Komplex der Formel Li2[Mo2O6(C2O4)] · 2 H2O (LMO) wurde dargestellt und durch chemische Analyse und IR-spektroskopisch charakterisiert. Die thermische Zersetzung dieses Komplexes wurde mittels TG und DTA untersucht. LMO verliert die zwei Wassermoleküle zwischen 75 und 170° unter Bildung des wasserfreien Produktes, das zwischen 240 und 380° in drei Stufen zersetzt wird. Die in den Temperaturbereich von 240–280° und 280–305° verlaufenden ersten zwei Reaktionsschritte ergeben Intermediäre der tentativen Zusammensetzung Li6[Mo6O19(C2O4)2] bzw. Li6[Mo6O20(C2O4)]. In dem sich bis 380° erstreckenden dritten Reaktionsschritt wird Li6[Mo6O20(C2O4)] unter Bildung des Endproduktes Li2Mo2O7 zersetzt.
A general and novel solution to the synthesis of biologically important stable analogues of prostacyclin PGI(2), namely benzindene prostacyclins, has been achieved via the stereoselective intramolecular Pauson-Khand cyclization (PKC). This work illustrates for the first time the synthetic utility and reliability of the asymmetric PKC route for synthesis and subsequent manufacture of a complex drug substance on a multikilogram scale. The synthetic route surmounts issues of individual step stereoselectivity and scalability. The key step in the synthesis involves efficient stereoselection effected in the PKC of a benzoenyne under the agency of the benzylic OTBDMS group, which serves as a temporary stereodirecting group that is conveniently removed via benzylic hydrogenolysis concomitantly with the catalytic hydrogenation of the enone PKC product. Thus the benzylic chiral center dictates the subsequent stereochemistry of the stereogenic centers at three carbon atoms (C(3a), C(9a), and C(1)). 相似文献
Summary The reactions of MCl3·3H2O (M=Ru, Rh or Ir) with hydrazones have been studied by three different methods and complexes of the types [M(LH2)(H2O)2]Cl3, [M(L)Cl(H2O)] and [M(LH2)Cl2]Cl·H2O have been isolated. Tentative structural conclusions are drawn for these products based upon elemental analysis, electrical conductance, magnetic moment, and i.r. and1H n.m.r. data. The thermal stability and mode of decomposition for the complexes have been studied by t.g.a., d.t.g. and d.s.c. techniques. 相似文献
Using Lobatto nodes, one-step methods of order six and eight have been obtained for the second-order differential equation y″ = f(x, y), y(x0) = y0, y′(x0) = y′0. The methods are shown to be P-stable. If , then at each integration step a system of dimension 3s, 4s, respectively, has to be solved. The numerical results, for two problems, obtained by using these methods are given in the end. 相似文献
A sensitive and inexpensive method of spectrophotometric determination of chromium(VI), based on the absorbance of its complex with malachite green and acetic acid at pH 2.5 is reported. The complex shows a molar absorptivity of 8 x 10(4) l.mole(-1) cm(-1) at 560 nm, using malachite green and acetic acid as reference solution. The effect of time, temperature, pH and reagent concentration is studied and optimum operating conditions are established. Beer's law is applicable in the concentration range 2.0-22.8 mug/ml chromium(VI). The resin beads act as a catalyst and as little as 1.6 mug of chromium(VI) is detected in the resin phase as compared to 4.1 mug in the solution phase. The standard deviation in the determinations is +/-0.40 mug/ml for a 10.35 mug/ml solution. 相似文献
Summary Ruthenium(III) complexes of types [Ru(L)3], [Ru(L)Cl(H2O)2], [Ru(L)Cl2]n, [Ru(L)Cl(H2O)]n(LH =Schiff bases derived from anthranilic acid and benzaldehyde, acetophenone, vanillin, cinnamaldehyde orm-hydroxyacetophenone; LH2=Schiff bases derived from anthranilic acid and salicylaldehyde oro-hydroxyacetophenone; LH=Schiff bases derived fromp-aminobenzoic acid and benzaldehyde, acetophenone, vanillin, cinnamaldehyde orm-hydroxyacetophenone; LH2=Schiff bases derived fromp-aminobenzoic acid and salicylaldehyde oro-hydroxyacetophenone) have been synthesized and characterized on the basis of elemental analyses, conductance, magnetic moment and spectral (electronic, i.r. and1H n.m.r.) data. The wavelengths of the principal electronic absorption peaks have been accounted for quantitatively in terms of crystal field theory and various parameters have been evaluated. On the basis of the electronic spectra, an octahedral geometry has been established for all these complexes except [Ru(L)Cl2]n. The complexes [Ru(L)Cl2]n are pentacoordinate and a trigonal-bipyramidal environment, D3h, is suggested for the ruthenium(III) ion. The thermal behaviour of these complexes has also been studied by t.g., d.t.g and d.s.c techniques. Heats of reaction for the decomposition steps were calculated from the d.s.c. curves. The antifungal and antiviral activities of the complexes with Schiff bases derived from anthranilic acid were also investigated. 相似文献
Suitably functionalized 3-carbomethoxy/cyano-2H-pyran-2-ones are excellent synthons for the synthesis of arenes and heteroarenes of therapeutic importance. The compounds 6-aryl-3-cyano-4-methylsulfanyl-2H-pyran-2-ones have been transformed into bridgedhead azolopyrimidines and imidazothiazines through thermal and base-induced ring transformation reactions with aminoazoles and imidazolidin-2-thiones, respectively. 相似文献