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211.
采用微波消解–原子荧光法测定PM2.5中砷、汞含量。实验结果表明,当还原剂硼氢化钾的质量分数为2%、溶液介质酸度为4%(体积分数)盐酸时,同时测定砷、汞可获得最佳的荧光值。砷、汞测定的检出限分别为0.027,0.006μg/L,空白滤膜的加标回收率分别为95.3%~101.7%,96.0%~106.0%,样品的加标回收率分别为95.0%~103.5%,93.3%~110.0%。该法检出限低,准确度高,适用于环境空气PM2.5中砷、汞含量的测定。 相似文献
212.
通过熔融扩散法合成了一系列不同含硫量的有序介孔碳(CMK-3)/硫复合材料(C x Sy).使用X射线衍射(XRD)、拉曼光谱(Raman)、比表面积测定仪(BET)、扫描电镜(SEM)、透射电镜(TEM)分析、表征和观察样品.将复合材料组装成钠硫电池,室温下测试电化学性能.循环伏安(CV)曲线结果表明,室温钠硫电池在1.61 V处有一个还原峰,对应于Na2Sx(x=2~5)的形成;在1.82 V和1.95 V分别有一个氧化峰,对应于Na2Sx(x=2~5)的分解.50%(by mass,下同)硫含量(C1S1)电极0.05C(1C=558 mA·g-1)倍率首周放电容量500 mAh·g-1,50周期循环比容量为305.6 mAh·g-1.交流阻抗数据拟合计算其表观活化能为21.83 kJ·mol-1.本研究可为室温钠硫电池多孔电极材料的研究提供一定的指导作用. 相似文献
213.
Xi‐Kai Shu Jia Li Feng Liu Xiao‐Jing Lin Xiao Wang Chun‐Xia Song 《Journal of separation science》2013,36(16):2680-2685
This study aimed to seek an efficient method to extract and purify yunaconitine and 8‐deacetylyunaconitine from Aconitum vilmorinianum Kom. by accelerated solvent extraction combined with pH‐zone‐refining counter‐current chromatography. The major extraction parameters for accelerated solvent extraction were optimized by an orthogonal test design L9 (3)4. Then a separation and purification method was established using pH‐zone‐refining counter‐current chromatography with a two‐phase solvent system composed of petroleum ether/ethyl acetate/methanol/water (5:5:2:8, v/v) with 10 mM triethylamine in the upper phase and 10 mM HCl in the lower phase. From 2 g crude extract, 224 mg of 8‐deacetylyunaconitine (I) and 841 mg of yunaconitine (II) were obtained with a purity of over 98.0%. The chemical structures were identified by ESI‐MS and 1H and 13C NMR spectroscopy. 相似文献
214.
The ultrafast excited state dynamics of trans-4-aminoazobenzene (trans-4-AAB) in ethanol was investigated by femtosecond transient absorption spectroscopy. After being excited to the S2 state by 400 nm, trans-4-AAB decays from the S2 state to the hot S1 state by internal conversion with time constant of -70 fs. The photoisomerization through inversion mechanism on the S1 potential energy surface and the internal conversion from the S1 state to the hot So state are observed, respectively. The average timescale of these two decay pathways is -0.7 ps. And the vibrational cooling of the hot So state of cis- and trans-4- AAB occur with time constants of -4 and N13 ps, respectively. Furthermore, the ultrafast intersystem crossing process are also observed. The timescale of intersystem crossing from the S2 state to the T4 state is about 480 ps while from the S1 state to the T2 state is -180 ps. 相似文献
215.
Prof. Dr. Minghuey Shieh Chun‐Hsien Yu Yen‐Yi Chu Yu‐Wen Guo Chung‐Yi Huang Kai‐Jieah Hsing Pei‐Chi Chen Chung‐Feng Lee 《化学:亚洲杂志》2013,8(5):963-973
The reactions of E powder (E=S, Se) with a mixture of Cr(CO)6 and Mn2(CO)10 in concentrated solutions of KOH/MeOH produced two new mixed Cr? Mn? carbonyl clusters, [E2CrMn2(CO)9]2? (E=S, 1 ; Se, 2 ). Clusters 1 and 2 were isostructural with one another and each displayed a trigonal‐bipyramidal structure, with the CrMn2 triangle axially capped by two μ3‐E atoms. The analogous telluride cluster, [Te2CrMn2(CO)9]2? ( 3 ), was obtained from the ring‐closure of Te2Mn2 ring complex [Te2Mn2Cr2(CO)18]2? ( 4 ). Upon bubbling with CO, clusters 2 and 3 were readily converted into square‐pyramidal clusters, [E2CrMn2(CO)10]2? (E=Se, 5 ; Te, 6 ), accompanied with the cleavage of one Cr? Mn bond. According to SQUID analysis, cluster 6 was paramagnetic, with S=1 at room temperature; however, the Se analogue ( 5 ) was spectroscopically proposed to be diamagnetic, as verified by TD‐DFT calculations. Cluster 6 could be further carbonylated, with cleavage of the Mn? Mn bond to produce a new arachno‐cluster, [Te2CrMn2(CO)11]2? ( 7 ). The formation and structural isomers, as well as electrochemistry and UV/Vis absorption, of these clusters were also elucidated by DFT calculations. 相似文献
216.
Der‐Lii M. Tzou Lin‐Kai Ni Mei‐Man Chen Min‐Chuan Chiou Li‐Chou Chen Shan‐Te Hsu Kuo‐Lung Ku Chien‐Chung Cheng 《中国化学会会志》2013,60(9):1107-1112
Solid‐state Nuclear Magnetic Resonance (ss‐NMR) 13C single‐pulse excitation spectroscopy in combination with the magic‐angle spinning (MAS) technique was applied to a series of Phalaenopsis tissues, including the leaf, sheath, stem, and root, at different growth and spiking periods. Compared with{1H}/13C cross‐polarization MAS spectra, the 13C single‐pulse excitation MAS spectra displayed very distinct spectral patterns, recognizable as fingerprints of the tissues studied. 1Here, we demonstrate that solid‐state 13C single‐pulse excitation NMR spectroscopy provides a direct and robust analytical tool for studying the various tissues of Phalaenopsis in different growth and spiking induction periods. 相似文献
217.
Yisheng Sun Zhao Zhao Qiangsheng Feng Qinqin Xu Longxian Lü Ji‐Kai Liu Ling Zhang Bin Wu Yong‐Quan Li 《Helvetica chimica acta》2013,96(1):76-84
Investigation of the cultured mycelia of Cordyceps ophioglossoides resulted in the isolation and characterization of three new unusual spiro[4.5]decane sesquiterpenes, cordycepol A ( 1 ), cordycepol B ( 2 ), and cordycepol C ( 3 ), and a new fumagillol analogue, cordycol ( 4 ). Their structures were established by spectroscopic means. The cytotoxic activities were also evaluated, compounds 3 and 4 showing their IC50 values in the range of 12–33 μg/ml against HeLa and HepG2 (Table 3). In addition, 3 and 4 were not obviously harmful towards normal liver cell lines LO2, showing IC50 values above 80 μg/ml. 相似文献
218.
An environmentally friendly process is reported for the palladium(II)‐catalyzed cyclofunctionalization of allylic hydroxylamine derivatives using a catalytic amount of copper(II) acetate and molecular oxygen as the cooxidant. 相似文献
219.
A general and efficient synthetic method of 1,3-bis(phenylseleno)-2-propanol by reducing diphenyl diselenides with sodium borohydride in basic environment and then reacting with epichlorohydrin are described. 相似文献
220.
Herein we report that LiAlH4/AlCl3 is a very efficient reagent for the reductive dehydration of aryl propargylic alcohols in tetrahydrofuran solvent at reflux to give 1,3-dienes with good yields and high E selection. The reaction conditions are mild and easy to operate, and a variety of aryl functional groups, such as bromo, fluoro, butyl, and methoxyl groups, are tolerated. With our protocol, useful (E,E)-1,3-dienes can be synthesized. Supplemental materials are available for this article. Go to the publisher's online edition of Synthetic Communications® to view the free supplemental file. 相似文献