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Design and Implementation of An RF Power Amplifier Used in Nuclear Magnetic Resonance Spectrometer
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LI You, MAO Wen-Ping, WANG Hui-Wang, LIU Yang, CHEN Fang, LIU Chao-Yang
Chinese Journal of Magnetic Resonance, 2011, 28(3): 326-338.
The design and implementation of a broadband RF power amplifier used in nuclear magnetic resonance spectrometer were introduced. Based on a two-stage architecture, the power amplifier was composed of a high frequency module, a broadband module and two directional couplers, to meet various requirements of NMR experiments. The rise time, fall time and power linearity of the power amplifier was measured on a home-built 500 MHz NMR spectrometer. Comparison of NMR sensitivity demonstrated good performance of this power amplifier in common NMR experiments.
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Spectral Analysis of Coal Tar from Xiaohuangshan Region
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MEI Yuan-Fei, ZHAO Xin, SUN Wan-Fu, TANG Jun, QIAO Ai-Xin
Chinese Journal of Magnetic Resonance, 2011, 28(3): 339-348.
The composition of coal tar from the Xiaohuangshan region, Xinjiang was studied by NMR spectroscopy and IR spectrometry. Structure parameters of the tar were calculated, and used to evaluate the degree of coalification and hydrocarbon generation capacity of the crude coal. The average aromatization-carbon ratio was found to be 0.78, carbon number (N ) 1.64, replace index (σ ) 0.49, and condensation index (Q )0.51. It was found that there were many alkyl-side chains connecting to the condensation aromatic nuclei, whose chain length was relatively short. Structural information was yielded from normalized and integrated IR spectra with the OPUS software. The parameters obtained from the NMR and IR spectra indicated that the crude coal was in medium metamorphic grade, and belonged to humic coal containing mainly vitrinite. According to the hydrocarbon generation mechanism, the gas potentiality of the coal tar was found to be better than oil, with its gas potential carbon mainly located in the methyl units. It was concluded that the coal from the Xiaohuangshan region can be used as the raw material to producing coal gas.
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Influence of Molecular Weight Distribution on Phase Transition and Self-Diffusion Behaviors of PNIPA/D2 O Solution
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RU Ge-Ying, LUO Jing-Ming, XU Yang-Lin, FENG Ji-Wen
Chinese Journal of Magnetic Resonance, 2011, 28(3): 349-356.
1 H NMR and self-diffusion NMR techniques were used to investigate the phase transition and diffusion property of two PNIPAs with different molecular weight distribution (MWD) in D2 O. It was found that MWD had significant influence on the phase transition and diffusion behaviors of PNIPAs. The broad-MWD PNIPA showed a smoothly decreased lower critical solution temperature (LCST)concentration curve, whereas the curve of the narrowMWD PNIPA decreased rapidly first, and then became flat. In the selfdiffusion experiments, the decay curve of the broad-MWD PNIPA showed a certain curvature, which became bigger and bigger with decreasing temperature and increasing concentration. But the decay curve of the narrow-MWD PNIPA was a nearly straight line, and the influences of temperature and concentration were minimal. Comparing the mean self-diffusion coefficient analyzed by a stretched exponential relation based on the classical Kohlrausch-Williams-Watts equation with that fitted with Equation (1), it could be shown that the former method is less susceptible to the influence of MWD.
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Synthesis and Spectroscopic Characterization of a Novel 1, 5-Dibenzodiazepine Derivative
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WANG Lu, PAN Xiang-Qiang, CAI Jing-Jing, ZU Jian-Ping
Chinese Journal of Magnetic Resonance, 2011, 28(3): 383-389.
Gallium (III) triflate-catalyzed reaction between o -phenylenediamine and ethyl propiolate under solvent-free and ultrasonic irradiation conditions produced a novel 1, 5-benzodiazepine derivative with a yield rate of 88%. Complete assignment of the 1 H and 13 C NMR chemical shift of the compound was obtained using 2D NMR techniques, including DEPT, 1 H-1 H COSY, 1 H-13 C HMQC and 1 H-13 C HMBC. Mass fragmentation pathway was proposed based on the high resolution MS spectrum of the compound.
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NMR Characterization of a Novel Curcumol Derivative
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CAO Xue, LI Yue-Qing, LIU Ji-Hong, ZHAO Wei-Jie
Chinese Journal of Magnetic Resonance, 2011, 28(3): 399-406.
The structure of curcumol was modified via a two-step reaction: exocyclic double bond oxidation and oxygen bridges acylation within the seven-membered ring. The reaction product was purified by silica gel column chromatography. Compound 2 was characterized by IR, ESI-MS, 1 H NMR, 13 C NMR and 2D NMR (i.e., gCOSY, gHSQC and gHMBC) techniques. The 1 H and 13 C NMR signals of compound 2 were assigned. Its structure was elucidated as 8-hydroxyl -12-isopropyl-2-methyl-tricyclo[6.2.2.01,5 ] dodecane-10-oxa-6, 9-dione.
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Structural Elucidation of Tectoruside Isolated from Iris tectorum Maxim. by NMR Spectroscopy
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YANG Yong-Xun, DONG Xiao-Ping, CHEN Hu-Lan
Chinese Journal of Magnetic Resonance, 2011, 28(3): 407-412.
The chemical constituents of Iris tectorum Maxim. were extracted with 95% alcohol, isolated by column chromatography on silica gel, and purified by recrystallization. The structures of the compounds were analyzed on the basis of the spectral data. A phenolic diglycoside, Tectoruside, was isolated from the n -Butanol portion of the extract, and its structure was elucidated by various spectroscopic data, including 2D NMR. The 1 H and 13 C NMR chemical shifts of the compounds were assigned. Its structure was found to be 1-{3′-methoxy-4′-[O-β-D- glucopyranosyl (1→6)-β -D -glucopyranosyl\]phenyl}ethanone.
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Two-Dimensional Localized Magnetic Resonance Spectroscopy and its In Vivo Application
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WANG Xiao-Hong, ZHANG Qin-Ta, LIN Yan-Qin, CHEN Zhong
Chinese Journal of Magnetic Resonance, 2011, 28(3): 419-436.
Localized magnetic resonance spectroscopy (MRS) is a non-invasive technique for acquiring in vivo biochemical and diagnostic information, acting as a powerful complement to MRI. It can provide important information for clinical diagnosis and disease prediction. However, 1D in vivo 1 H MRS has the problems of peak crowding, low spectral resolution and difficult peak identification. The twodimensional (2D) MRS has been introduced to address these problems to a large extent. In this review, we analyzed the advantages and disadvantages of several typical 2D MRS methods. Their in vivo applications in brain, muscle, breast and prostates were also discussed. Although 2D MRS has the limitation of long experimental time, it still holds some unique advantages and presents a promising prospect according to the latest research.