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41.
Complexes of Dioxocyanogen (OCN)2 with TiCl4 and ZrCl4 A solution of (OCN)2 was obtained by reaction of AgOCN with Br2 in H2CCl2 at ?70°C. From this the complexes TiCl4(NCO)2 and ZrCl4(NCO)2 were obtained by addition of equimolar amounts of TiCl4 and ZrCl4, respectively. According to the i.r. and Raman spectra, the (NCO)2 ligand is bonded via its N atoms to the metal.  相似文献   
42.
A rapid and sensitive method for the analysis of delta9-tetrahydrocannabinol (THC) in preserved oral fluid was developed and fully validated. Oral fluid was collected with the Intercept, a Food and Drug Administration (FDA) approved sampling device that is used on a large scale in the U.S. for workplace drug testing. The method comprised a simple liquid-liquid extraction with hexane, followed by liquid chromatography-tandem mass spectrometry (LC-MS-MS) analysis. Chromatographic separation was achieved using a XTerra MS C18 column, eluted isocratically with 1 mM ammonium formate-methanol (10:90, v/v). Selectivity of the method was achieved by a combination of retention time, and two precursor-product ion transitions. The use of the liquid-liquid extraction was demonstrated to be highly effective and led to significant decreases in the interferences present in the matrix. Validation of the method was performed using both 100 and 500 MicroL of oral fluid. The method was linear over the range investigated (0.5-100 ng/mL and 0. 1-10 ng/mL when 100 and 500 microL, respectively, of oral fluid were used) with an excellent intra-assay and inter-assay precision (relative standard deviations, RSD <6%) for quality control samples spiked at a concentration of 2.5 and 25 ng/mL and 0.5 and 2.5 ng/mL, respectively. Limits of quantification were 0.5 and 0.1 ng/mL when using 100 and 500 microL, respectively. In contrast to existing GC-MS methods, no extensive sample clean-up and time-consuming derivatisation steps were needed. The method was subsequently applied to Intercept samples collected at the roadside and collected during a controlled study with cannabis.  相似文献   
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The synthesis of nanostructured poly(N-isopropylacrylamide) (polyNIPA) hydrogels by a two-stage polymerization process is reported here. The process involves the synthesis of slightly crosslinked polyNIPA nanoparticles by inverse (w/o) microemulsion polymerization; then, these particles are dried, cleaned and dispersed in an aqueous solution of NIPA and a crosslinking agent (N,N-methylene-bis-acrylamide or NMBA) and polymerized to produce the nanostructured hydrogels. Their swelling and de-swelling kinetics, volume phase transition temperatures (T VPT) and mechanical properties at the equilibrium swollen state are investigated as a function of the weight ratio of polyNIPA particles to monomer (NIPA). The nanostructured gels exhibit larger equilibrium water uptake, faster swelling and de-swelling rates and similar T VPT than those of the conventional ones; moreover, the elastic and Young moduli are larger than those of the conventional hydrogels at similar swelling ratios. The fast swelling and de-swelling kinetics are explained in terms of the controlled inhomogeneities introduced by the method of synthesis.  相似文献   
44.
Fernandez L  Olsina R 《Talanta》1992,39(12):1605-1609
The operating conditions for the absorptiometric determination of Yb(III) with the reagent 2-(3,5-dichloro-2-pyridylazo)-5-dimethylaminophenol (3,5-diClDMPAP) by a liquid—liquid extraction technique are presented. The complex yields a molar absorptivity of 1.54 × 105l.mole−1.cm−1max = 588 nm) and an optimum concentration range of 0.025–1.360n mg/l., at pH = 10. The method developed has been applied to the determination of Yb(III) in synthetic and concrete mixtures.  相似文献   
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We present a neutron scattering study carried out on single-crystals of the magnetoelectric compound GaFeO3, prepared by the floating-zone (FZ) method. The refinement of the crystal structure indicates the existence of a large amount of iron on the gallium site, corresponding to a strong internal substitution disorder. We show that the Ga/Fe disorder and the magnetic transition temperature are weakly dependent on the growth conditions. The disorder also affects the magnetic excitations; our measurements evidence damped spin waves, well defined only close to the Brillouin zone centre.  相似文献   
49.
The spatial discretization of unsteady incompressible Navier–Stokes equations is stated as a system of differential algebraic equations, corresponding to the conservation of momentum equation plus the constraint due to the incompressibility condition. Asymptotic stability of Runge–Kutta and Rosenbrock methods applied to the solution of the resulting index‐2 differential algebraic equations system is analyzed. A critical comparison of Rosenbrock, semi‐implicit, and fully implicit Runge–Kutta methods is performed in terms of order of convergence and stability. Numerical examples, considering a discontinuous Galerkin formulation with piecewise solenoidal approximation, demonstrate the applicability of the approaches and compare their performance with classical methods for incompressible flows. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   
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