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71.
Hans-Rudolf Buser Michael Oehme Walter Vetter Bernd Luckas 《Fresenius' Journal of Analytical Chemistry》1993,347(12):502-512
Summary Conventional electron ionization (EI) mass spectrometry (MS) and MS/MS techniques were applied to the analysis of two abundant octa and nonachlorobornanes isolated from seals of the Baltic sea and originating from technical toxaphene. The exact sterical structures of the two compounds were previously determined using nuclear magnetic resonance (NMR) spectroscopy by two independent research groups. The MS and MS/MS data generated in this study allowed partial structure elucidation of these polychlorobornanes, in particular revealing the distribution of the Cl substituents between the six-membered carbon ring, the bridge and the bridgehead in the parent bornane structure. Fragmentation of the six-membered carbon ring and the bridge by retro-Diels-Alder (RDA) and related mechanisms was discovered by studying specific parent/daughter ion transitions. The detailed fragmentation pathways formulated may be applicable to the structure elucidation of other toxaphene congeners and the monitoring of strategic transitions is highly selective for the detection of these compounds in technical toxaphene and in environmental samples. 相似文献
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Yu. V. Belovitskaya I. V. Pekov E. R. Gobechiya N. A. Yamnova Yu. K. Kabalov N. V. Chukanov J. Schneider 《Crystallography Reports》2002,47(2):223-228
The crystal structures of two ancylite specimens from Khibiny massif (the Kola Peninsula, Russia)—ancylite-(Ce) from alkali hydrothermalites (Sr1.01Ca0.02Ba0.01)Σ1.04(Ce0.52La0.28Nd0.11Pr0.04 Sm0.01)Σ0.96(CO3)2(OH0.83F0.13)Σ0.96 · 0.9H2O and ancylite-(Ce) from carbonatites—have (Sr0.80Ca0.05Ba0.01)Σ0.86(Ce0.62La0.40Nd0.09Pr0.03) Σ1.14(CO3)2(OH0.99F0.15)Σ1.14 · 1.0H2O been refined by the Rietveld method. A focusing STOE-STADIP diffractometer with a bent Ge(111) primary monochromator was used (λ MoK α 1 radiation, 2.16° < 2θ < 54.98°; reflection number 237–437). All the computations for ancylite from alkali hydrothermalites were performed within the sp. gr. Pmc21, a = 5.0634(1) Å, b = 8.5898(1) Å, c = 7.2781(1) Å, V = 316.55(1) Å3, R wp = 1.90; the computations for ancylite from carbonatites were performed within the sp. gr. Pmcn, a = 5.0577(1) Å, b = 8.5665(2) Å, c = 7.3151(2) Å, V = 316.94(1) Å3, R wp = 2.38 in the anisotropic approximation of thermal vibrations of cations and oxygen atoms. 相似文献
74.
B. MacMillan M. Halse M. Schneider L. Fardy Y. H. Chui B. J. Balcom 《Applied magnetic resonance》2002,22(2):247-256
Magnetic resonance imaging has rarely been applied to rigid polymeric materials, due primarily to the strong dipolar coupling and short signal lifetimes inherent in these materials. SPRITE (single point ramped imaging withT 1 enhancement) (B. J. Balcom, R. P. MacGregor, S. D. Beyea, D. P. Green, R. L. Armstrong, T. W. Bremner: J. Magn. Reson. A123, 131–134, 1996) is particularly well suited to imaging solid materials. With SPRITE, the only requirement is thatT 2* be long enough so that the signal can be phase-encoded. The minimum phase encoding time is limited by the maximum gradient strength available and by the instrument deadtime. At present this is usually tens of microseconds and will only improve with refinements in technology. We have used the SPRITE sequence in conjunction with raising the sample temperature to obtain images of rigid polymers that have largely frustrated conventional imaging methods. This approach provides a straightforward and reliable method for imaging a class of samples that, up until now, have been very difficult to image. 相似文献
75.
Convective heat transfer from an array of small, cylindrical bodies of arbitrary shape in an unbounded, two-dimensional domain is a singular perturbation problem involving an infinite logarithmic expansion in the small parameter ε, representing the order of magnitude of the size of the bodies. Using the method of matched asymptotic expansions, we formulate a hybrid asymptotic-numerical method to solve for the dimensionless, steady-state temperature. We assume that the velocity field of the fluid surrounding the bodies is arbitrary but known. From our asymptotic solution for an arbitrary velocity field, we present the results for two special cases: a uniform flow field and a simple shear flow field. We demonstrate the asymptotic results of the hybrid method through a number of examples and, in a particular case, we compare these results to an exact analytical solution. 相似文献
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78.
Using topological methods we give a proof that the free product of two strict subgroup separable groups with infinite cyclic amalgamation is subgroup separable. 相似文献
79.
Daria E. Lonsdale Geoffrey Johnston‐Hall Amanda Fawcett Craig A. Bell Carl N. Urbani Michael R. Whittaker Michael J. Monteiro 《Journal of polymer science. Part A, Polymer chemistry》2007,45(16):3620-3625
In this work, we propose that retardation in vinyl acetate polymerization rate in the presence of toluene is due to degradative chain transfer. The transfer constant to toluene (Ctrs) determined using the Mayo method is equal to 3.8 × 10?3, which is remarkably similar to the value calculated from the rate data, assuming degradative chain transfer (2.7 × 10?3). Simulations, including chain‐length‐dependent termination, were carried out to compare our degradative chain transfer model with experimental results. The conversion–time profiles showed excellent agreement between experiment and simulation. Good agreement was found for the Mn data as a function of conversion. The experimental and simulation data strongly support the postulate that degradative chain transfer is the dominant kinetic mechanism. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 3620–3625, 2007 相似文献
80.