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81.
82.
Different substituents have been introduced into the 5-position of 2-t-butoxythiophene and by subsequent acid-catalyst dealkylation the corresponding hydroxythiophenes (or their different tautomeric forms) have been isolated in high yields. By NMR, IR and UV-spectroscopy the constitution and the composition of the different tautomeres have been determined. The reaction between carbonyl compounds and 5-t-butoxy-2-thiophenelithium gives carbinols, which upon heating with p-toluenesulphonic acid yielded 5-methylene-3-thiolen-2-ones. 相似文献
83.
The 31P? 31P and 13C? 31P coupling constants in 1,6-diphosphatriptycene have been obtained from analysis of its proton decoupled 13C n.m.r. spectra. More accurate data, however, resulted from simultaneous analysis of the proton decoupled 13C spectra and 31P(13C) satellite spectra. The 13C? 31P couplings are strongly influenced by the proximity and orientation of the phosphorus lone pair electrons. The first 31P? 31P coupling in an aromatic diphosphine is reported. 相似文献
84.
N Sulphonylformamidines have been prepared in a CuCl catalysed α-addition reaction between sulphonamides and isocyanides. The actual tautomeric form present has been shown to be the N2 sulphonyl-formamidine by 13C NMR spectroscopy. Variable temperature NMR experiments show the existence of two rotamers. 相似文献
85.
59Co triple-quantum (3Q) MAS and single-pulse MAS NMR spectra of K3Co(CN)6 have been obtained at 14.1 T and used in a comparison of these methods for determination of small chemical shift anisotropies for spin I = 7/2 nuclei. From the 3QMAS NMR spectrum a spinning sideband manifold in the isotropic dimension with high resolution is reconstructed from the intensities of all spinning sidebands in the 3QMAS spectrum. The chemical shift anisotropy (CSA) parameters determined from this spectrum are compared with those obtained from MAS NMR spectra of (i) the complete manifold of spinning sidebands for the central and satellite transitions and of (ii) the second-order quadrupolar lineshapes for the centerband and spinning sidebands from the central transition. A good agreement between the three data sets, all of high precision, is obtained for the shift anisotropy (delta(sigma) = delta(iso) - delta(zz)) whereas minor deviations are observed for the CSA asymmetry parameter (eta(sigma)). The temperature dependence of the isotropic 59Co chemical shift has been studied over a temperature range from -28 to +76 degrees C. A linear and positive temperature dependence of 0.97 ppm/degree C is observed. 相似文献
86.
First we introduce and analyze a convergent numerical method for a large class of nonlinear nonlocal possibly degenerate convection diffusion equations. Secondly we develop a new Kuznetsov type theory and obtain general and possibly optimal error estimates for our numerical methods—even when the principal derivatives have any fractional order between 1 and 2! The class of equations we consider includes equations with nonlinear and possibly degenerate fractional or general Levy diffusion. Special cases are conservation laws, fractional conservation laws, certain fractional porous medium equations, and new strongly degenerate equations. 相似文献
87.
Jannike Solsvik Hugo A. Jakobsen 《Journal of Dispersion Science and Technology》2014,35(11):1626-1642
In the churn-turbulent bubbly flow regime with highly nonuniform bubble size distributions, bubble breakage and coalescence are important processes because they govern the bubble size distribution and consequently directly affect the interfacial mass, momentum, and heat transfer fluxes through the renewal bubble surfaces. At present, accurate prediction of bubble size distributions of dispersed gas–liquid flows by use of the population balance (PB) equation is a difficult task. The modeling of bubble breakup and coalescence rates is very complex and is based on the knowledge of collision and breakup frequencies, breakage daughter size distributions, and probability of coalescence. In this work, we focus on the coalescence phenomenon. The coalescence models are still on an empirical level and the mechanisms are not fully understood. This motivates the analysis of the suitability of the coalescence closures for the prediction of experimental data obtained from coalescence dominated gas–liquid flows. For this task, a cross-sectional averaged combined multifluid-PB model is adopted. Based on different theories for the coalescence efficiency, the simulation results show a similar trend in the prediction of the experimental data. Good prediction of the Sauter mean diameter is achieved although the shape of the bubble size distribution is not completely reproduced. The second aim of this work is to review the PB framework. Here, focus is placed on the coalescence term and the combined multifluid-PB model based on kinetic theory approach. 相似文献
88.
C. Gainaru M. Wikarek S. Pawlus M. Paluch R. Figuli M. Wilhelm T. Hecksher B. Jakobsen J. C. Dyre R. Böhmer 《Colloid and polymer science》2014,292(8):1913-1921
The monohydroxy alcohol 5-methyl-3-heptanol is studied using rheology at ambient pressure and using dielectric spectroscopy at elevated pressures up to 1.03 GPa. Both experimental techniques reveal that the relaxational behavior of this liquid is intermediate between those that show a large Debye process, such as 2-ethyl-1-hexanol, or a small Debye-like feature, such as 4-methyl-3-heptanol, with which comparisons are made. Various phenomenological approaches assigning a time scale for the rheological signature of supramolecular dynamics in monohydroxy alcohols are discussed. 相似文献
89.
Quantification of physiological levels of vitamin D3 and 25‐hydroxyvitamin D3 in porcine fat and liver in subgram sample sizes 下载免费PDF全文
Anders Burild Henrik L. Frandsen Morten Poulsen Jette Jakobsen 《Journal of separation science》2014,37(19):2659-2663
Most methods for the quantification of physiological levels of vitamin D3 and 25‐hydroxyvitamin D3 are developed for food analysis where the sample size is not usually a critical parameter. In contrast, in life science studies sample sizes are often limited. A very sensitive liquid chromatography with tandem mass spectrometry method was developed to quantify vitamin D3 and 25‐hydroxyvitamin D3 simultaneously in porcine tissues. A sample of 0.2–1 g was saponified followed by liquid–liquid extraction and normal‐phase solid‐phase extraction. The analytes were derivatized with 4‐phenyl‐1,2,4‐triazoline‐3,5‐dione to improve the ionization efficiency by electrospray ionization. The method was validated in porcine liver and adipose tissue, and the accuracy was determined to be 72–97% for vitamin D3 and 91–124% for 25‐hydroxyvitamin D3. The limit of quantification was <0.1 ng/g, and the precision varied between 1.4 and 16% depending on the level of spiking. The small sample size required for the described method enables quantification of vitamin D3 and 25‐hydroxyvitamin D3 in tissues from studies where sample sizes are limited. 相似文献
90.
Nina Munkholt Jakobsen Michael Sørensen 《Stochastic Processes and their Applications》2019,129(9):3282-3318
Asymptotic theory for approximate martingale estimating functions is generalised to diffusions with finite-activity jumps, when the sampling frequency and terminal sampling time go to infinity. Rate-optimality and efficiency are of particular concern. Under mild assumptions, it is shown that estimators of drift, diffusion, and jump parameters are consistent and asymptotically normal, as well as rate-optimal for the drift and jump parameters. Additional conditions are derived, which ensure rate-optimality for the diffusion parameter as well as efficiency for all parameters. The findings indicate a potentially fruitful direction for the further development of estimation for jump–diffusions. 相似文献