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1.
2.
The crystal structures of α-UF5 and U2F9 were refined with high-resolution neutron powder diffraction data from an mixture. Refinement was achieved by a multiphase Rietveld profile refinement technique. The results are compared with previous X-ray and neutron powder studies. 相似文献
3.
High resolution 13C and 15N NMR spectra have been obtained for powdered CH3CN. The presence of resolved dipolar structure in the 13C spectra permits the conclusion that the symmetry axis of the 13C shielding tensor lies along the CN bond direction. 相似文献
4.
Sulfur hexafluoride has a body-centered cubic phase (a = 5.915(3) Å) between its melting point (222.4°K) and 93°K, below which a lower symmetry phase exists. NMR studies show that in both phases there is rapid reorientation of the sulfur hexafluoride molecules. From a neutron diffraction pattern collected at 193°K with λ = 1.086 Å, the data were not satisfied by a model with a spherically symmetrical fluorine density nor by a refinement with conventional ellipsoidal-shaped atoms. The latter gave systematically low S-F distances and abnormally high βij thermal factors. Good agreement was obtained by a combination of Kubic Harmonics with full-matrix least-squares analysis of the neutron profile pattern. The refinement was made with one variable Kubic Harmonic coefficient a2 = 5.94(11), with and . Only four least-squares variables were required with 225 observations in the range of one or more hkl reflections to 2θ = 58.3°. AS-F distance of 1.542(4) Å, obtained from the neutron diffraction data, is in good agreement with the reported value of 1.564(10) Å found from electron diffraction measurements of the vapor. The disordered fluorine distribution has broad maxima on the cell edges similar to those found in the plastic cubic phases of MoF6 and WF6. 相似文献
5.
Russell J. Waugh John H. Bowie Roger N. Hayes 《Journal of mass spectrometry : JMS》1991,26(4):250-256
Deprotonated dipeptides, on collisional activation, fragment by the characteristic process NH2CH(R1) CONHCH(R2)CO2? → NH2?C(R1)CONHCH(R2)CO2H → ?NHCH(R2)CO2H + NH2C(R1)?C?O, when R1 and R2 = H or alkyl. However, when one of the constituent amino acids is either aspartic acid or glutamic acid, the standard cleavage becomes minor in comparison with fragmentation through the α-side-chain of Asp or Glu. For example, [Asp-Leu - H]? and [Leu-Asp - H]? both fragment principally by loss of water, a fragmentation not normally noted for peptides. In addition, [Leu-Asp - H]? loses CO2 and also forms HO2CCH?CHCO2?˙. These fragmentations establish that Asp is the C-terminal amino acid. In contrast, isomeric Glu dipeptides, e.g. [Glu-Ala - H]? and [Ala-Glu - H]? undergo similar fragmentation, both competitively losing H2O and CO2. Both spectra also contain a product ion at m/z 128, identified as the pyroglutamate anion. Product ion and deuterium-labelling studies have been used in an attempt to elucidate the complex fragmentation mechanisms in these systems. 相似文献
6.
7.
Verónica de la Fuente Dipl.‐Chem. Mark Waugh Dr. Graham R. Eastham Dr. Jonathan A. Iggo Dr. Sergio Castillón Prof. Dr. Carmen Claver Prof. Dr. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2010,16(23):6919-6932
Novel cis‐1,2‐bis(di‐tert‐butyl‐phosphinomethyl) carbocyclic ligands 6 – 9 have been prepared and the corresponding palladium complexes [Pd(O3SCH3)(L‐L)][O3SCH3] (L‐ L=diphosphine) 32 – 35 synthesised and characterised by NMR spectroscopy and X‐ray diffraction. These diphosphine ligands give very active catalysts for the palladium‐catalysed methoxycarbonylation of ethene. The activity varies with the size of the carbocyclic backbone, ligands 7 and 9 , containing four‐ and six‐membered ring backbones giving more active systems. The acid used as co‐catalyst has a strong influence on the activity, with excess trifluoroacetic acid affording the highest conversion, whereas excess methyl sulfonic acid inhibits the catalytic system. An in operando NMR spectroscopic mechanistic study has established the catalytic cycle and resting state of the catalyst under operating reaction conditions. Although the catalysis follows the hydride pathway, the resting state is shown to be the hydride precursor complex [Pd(O3SCH3)(L‐ L)][O3SCH3], which demonstrates that an isolable/detectable hydride complex is not a prerequisite for this mechanism. 相似文献
8.
R. Waugh 《Journal of sound and vibration》1984,93(2):289-305
A computer was programmed to model the distributions of dB(A) levels reaching the ears of an imaginary workforce wearing hearing protectors selected on the basis of either octave band attenuation values or various simplified ratings in use in Australia, Germany, Poland, Spain or the U.S.A. Both multi-valued and single-valued versions of dB(A) reduction and sound level conversion ratings were considered. Ratings were compared in terms of precision and protection rate and the comparisons were replicated for different samples of noise spectra (N = 400) and hearing protectors (N = 70) to establish the generality of the conclusions. Different countries adopt different approaches to the measurement of octave band attenuation values and the consequences of these differences were investigated. All rating systems have built-in correction factors to account for hearing protector performance variability and the merits of these were determined in the light of their ultimate effects on the distribution of dB(A) levels reaching wearers' ears. It was concluded that the optimum rating is one that enables the dB(A) level reaching wearers to be estimated by subtracting a single rating value from the dB(C) level of the noise environment, the rating value to be determined for a pink noise spectrum from mean minus one standard deviation octave band attenuation values with further protection rate adjustments being achieved by the use of a constant correction factor. 相似文献
9.
Enhancement of the surface properties of a material by means of laser radiation has been amply demonstrated previously. In this work a comparative study for the surface modification of nylon 6,6 has been conducted in order to vary the wettability characteristics using CO2 and excimer lasers. This was done by producing 50 μm spaced (with depths between 1 and 10 μm) trench-like patterns using various laser parameters such as varying the laser power for the CO2 laser and number of pulses for the excimer laser. Topographical changes were analysed using optical microscopy and white light interferometry which indicated that both laser systems can be implemented for modifying the topography of nylon 6,6. Variations in the surface chemistry were evaluated using energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy analysis which showed that the O2 increased by up to 1.5 at% and decreased by up to 1.6 at% for the CO2 and F2 laser patterned samples, respectively. Modification of the wettability characteristics was quantified by measuring the advancing contact angle, which was found to increase in all instances for both laser systems. Emery paper roughened samples were also analysed in the same manner to determine that the topographical pattern played a major role in the wettability characteristics of nylon 6,6. From this, it is proposed that the increase in contact angle for the laser processed samples is due to a mixed intermediate state wetting regime owed to the periodic surface roughness brought about by the laser-induced trench-like topographical patterns. 相似文献
10.
Simon J. Illingworth Iain C. Waugh Matthew P. Juniper 《Proceedings of the Combustion Institute》2013,34(1):911-920
This paper examines nonlinear thermoacoustic oscillations of a ducted Burke-Schumann diffusion flame. The nonlinear dynamics of the thermoacoustic system are studied using two distinct approaches. In the first approach, a continuation analysis is performed to find limit cycle amplitudes over a range of operating conditions. The strength of this approach is that one can characterize the coupled system’s nonlinear behaviour over a large parameter space with relative ease. It is not able to give physical insight into that behaviour, however. The second approach uses a Flame Describing Function (FDF) to characterize the flame’s response to harmonic velocity fluctuations over a range of forcing frequencies and forcing amplitudes, from which limit cycle amplitudes can be found. A strength of the FDF approach is that it reveals the physical mechanisms responsible for the behaviour observed. However, the calculation of the FDF is time consuming, and it must be recalculated if the flame’s operating conditions change. With the strengths and shortcomings of the two approaches in mind, this paper advocates combining the two to provide the dynamics over a large parameter space and, furthermore, physical insight into that behaviour at judiciously-chosen points in the parameter space. Further physical insight concerning the flame’s near-linear response at all forcing amplitudes is given by studying the forced flame in the time domain. It is shown that, for this flame model, the limit cycles arise because of the flame’s nonlinear behaviour when it is close to the inlet. 相似文献