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Precision and sensitivity optimization of quantitative measurements in solid state NMR 总被引:2,自引:1,他引:1
Ziarelli F Viel S Sanchez S Cross D Caldarelli S 《Journal of magnetic resonance (San Diego, Calif. : 1997)》2007,188(2):260-266
This work presents a methodology for optimizing the precision, accuracy and sensitivity of quantitative solid state NMR measurements based on the external reference method. It is shown that the sample must be exclusively located within and completely span the coil region where the NMR response is directly proportional to the sample amount. We describe two methods to determine this "quantitative" coil volume, based on whether the probe is equipped or not with a gradient coil. In addition, to improve the sensitivity and the accuracy, an optimum rotor packing design is described, which allows the sample volume of the rotor to be matched to the quantitative coil volume. Experiments conducted on adamantane and NaCl, which are representative of a soft and hard material, respectively, show that one order of magnitude increase in experimental precision can be achieved with this methodology. Interestingly, the precision can be further improved by using the ERETIC method in order to compensate for most instrumental instabilities. 相似文献
84.
一个跨音风扇级转/静干扰流动的时间精确模拟 总被引:5,自引:1,他引:4
本文采用双时间步法,较为方便地将孤立叶排定常流场求解拓广为转/静干扰非定常流场时间精确求解,而且该流场时间精确求解方法收敛速度较作者最初工作有较大提高.文章通过对一跨音风扇级非定常流场时间精确模拟,对叶轮机非定常流动建立了一定理解. 相似文献
85.
The title reaction has been used as an example to test the importance of using a hindered rotor treatment instead of a harmonic oscillator model for calculating vibrational partition functions corresponding to low-frequency internal rotation modes. First, a normal-mode analysis according to the Ayala and Schlegel's algorithm has been used to identify the internal rotation modes of methanethiol and the transition state structure. Then, after calculation of the energy barrier for each internal rotation, the corresponding hindered rotor partition functions have been calculated following the CW scheme of Chuang and Truhlar. The results show that the anharmonic treatment produces a rather modest improvement of the rate constants at room temperature or below. 相似文献
86.
In this study, we examined the gas-phase pyrolysis of ethyl N,N-dimethylcarbamate theoretically at various theoretical levels. The reaction consists of a two-step mechanism, with N,N-dimethylcarbamic acid and ethylene as reaction intermediates. In the first step, the reaction proceeds via a six-membered cyclic transition state (TS), which is more favorable than that via a four-membered cyclic TS. Here, the contribution of entropy to the overall potential energy surface was found to play an important role in determining the rate-limiting step, which was found to be the second step when viewed in terms of the enthalpy of activation (DeltaH(not equal)), but the first step when entropy changes (-TDeltaS(not equal)) were considered. These results are consistent with experimental findings. Moreover, the experimental activation entropy can be reproduced by using the hindered rotor approximation, which converts some low vibration frequencies that correspond to internal rotational modes into hindered rotors. 相似文献
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89.
Ding Yuan Ting Wu Rong-yuan Chen Gui-zhen Zhang 《Journal of Macromolecular Science: Physics》2018,57(5):348-363
The properties of polymer matrix composites are related not only to the chemical composition of the materials but also to the processing equipment used for their preparation which has a direct influence on the microstructure of the composites. In this paper polypropylene (PP)/multi-walled carbon nanotubes (MWCNTs) nanocomposites were prepared by melt blending through a self-developed, eccentric rotor extruder (ERE). The structure and elongational deformation mechanism of an ERE were described in detail. The morphological, rheological, thermal and mechanical properties of the resulting PP/MWCNTs nanocomposites were investigated. Scanning electron microscopy (SEM) and rheological analysis showed that the MWCNTs were well dispersed in the PP matrix. The thermal stability was investigated by thermogravimetric analysis (TGA) and indicated that the addition of MWCNTs could effectively improve the thermal stability of pure PP. The percentage of crystallinity and tensile strength of the composites were improved as a result of the heterogeneous nucleation effect of the MWCNTs in the PP matrix. The research results revealed that the enhancement of the properties of PP/MWCNTs composites could be attributed to a better dispersion of the MWCNTs in the matrix as compared to samples prepared by conventional extrusion. 相似文献
90.
《Comptes Rendus Physique》2017,18(1):31-46
This paper reviews the physics of quantum disorder in relation with a series of experiments using laser-cooled atoms exposed to “kicks” of a standing wave, realizing a paradigmatic model of quantum chaos, the kicked rotor. This dynamical system can be mapped onto a tight-binding Hamiltonian with pseudo-disorder, formally equivalent to the Anderson model of quantum disorder, with quantum chaos playing the role of disorder. This provides a very good quantum simulator for the Anderson physics. 相似文献