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51.
2,2'-二乙炔基-1,1'-联萘为模板构筑的新的环芳化合物的合成及其光学性质 总被引:1,自引:0,他引:1
基于2,2'-二取代的联萘衍生物在手性构型上高度稳定的特点,分别以光学活性的(R)-和(S)-2,2'-二乙炔基-1,1'-联萘为模板,设计了2个有趣的拓扑环芳分子四联萘笼状对映异构体(R,R,R,R)-2和(S,S,S,S)-2.其合成路线涉及保护基的控制导入、苯连接桥的链接、保护基的脱去以及偶合成环反应4个步骤.用MS,IR,UV-Vis,1HNMR,13CNMR和元素分析等技术对其进行了表征,并比较了其光学性质.研究结果表明,采用这种模板合成方法能够有效地获得具有单一手性的目标化合物.镜像特征的圆二色(CD)谱和比旋光度[α]D的测定结果清楚地反映了它们的对映异构关系. 相似文献
52.
Ponce De León CA Montes Bayón M Caruso JA 《Analytical and bioanalytical chemistry》2002,374(2):230-234
Vitamin E supplements are either isolated from plants sources or prepared synthetically. Isolation from plants includes eight different tocopherol structures. Vitamin E synthesis includes seven different stereoisomers, which involves the use of several catalysts that may lead to trace element contamination in the vitamin. The use of ICP-MS is an ideal technique for detecting these trace elements. However, the oily nature of the samples requires the development of a sample preparation methodology. This study was done upon the request of synthetic vitamin E manufacturers to test the trace metal purity of their samples. In this work, the comparison of an acid microwave digestion and emulsion preparation is discussed. Cromium, nickel, tin and lead were found in the synthetic vitamin E analyzed and 200, 60, 9 and 45 ppb were the concentrations found respectively for these elements.Digesting the samples gives slightly lower detection limits compared to the emulsion preparation. 相似文献
53.
Zn-Al-Ce三元类水滑石的制备及性质研究 总被引:8,自引:1,他引:8
采用共沉淀法,水热合成层状化合物一硝酸根柱撑锌铝铈三元类水滑石,分别测定了各种单一金属盐溶液及M^2 /M^3 摩尔比为2,Ce^3 /Al^3 摩尔比为0.25的混合金属盐的NaOH滴定曲线,并利用XRD对不同条件下合成产物进行物相分析。实验结果表明:在M^2 /M^2 =2,Ce^3 /Al^3 =0.07~0.50,pH=5.8~6.5条件下进行多种离子共沉淀,并经120℃、6h水热处理后,均能合成结构单一的ZnAlCe—HTLLcs,利用TG—DTlA、FT—IR、ICP对合成物进行了表征,筛选出适宜的合成条件,并对HTLcs层状结构的热行为进行初步研究,结果表明ZnAlCe—HTLcs热稳定性较差,层间结合水、层板羟基及层间客体物种(NO3^-)失去温度在240℃左右,易于转化为复合氧化物,将此复合氧化物应用于NO的催化?肖除反应,680℃下NO的转化率高达近100%。 相似文献
54.
A new Sequiterpenoid from Eupatorium adenophorum Spreng 总被引:1,自引:0,他引:1
A new sequiterpenoid compound 8aα-hydroxy-1-isopropyl-4,7-dimethyl-1,2,3,4,6,8a-hexahydro-naphthalene-2,6-dione(1),together with seven known compounds anti-HH-dimer-coumarin(2),(-)-5-exo-hydroxy-bomeol(3),O-hydroxyl cinnamic acid(4),9β-hydroxy-ageraphorone(5),10Hα-9-oxo-ageraphorone(6),10Hβ-9-oxo-ageraphorone(7)and 9-oxo-10,11-dehydroageraphorone 8,was isolated from the leaves of Eupatorium adenopho-rum Spreng.The structures were elucidated by IR,~1H and ~(13)C NMR,EIMS,HMBC and single-crystal X-ray spec-tral data. 相似文献
55.
Porous anodic alumina (PAA) was used as a template to prepare Co nanowires array from 1-ethyl-3-methylimidazolium chloride ionic liquid by direct current method. The surface morphology of porous anodic alumina template was observed by field emission-scanning tunneling microscopy (FE-SEM) before and after the electrodeposition of Co nanowires. The electrodeposition of Co nanowires was characterized by transmission electron microscopy (TEM) and X-ray powder diffraction (XRD). TEM results indicate that the Co nanowire surface is coarse and porous when aqueous solution was used as electrolyte, and the Co nanowire deposited from the ionic liquid is uniform and smooth. XRD results show that the electrodeposition of Co is a mixture of crystal and microcrystal phase. 相似文献
56.
通过原子转移自由基聚合方法, 在丁酮/异丙醇混合溶剂中合成了分子量可控和分布较窄的聚丙烯酸叔丁酯-b-聚N-异丙基丙烯酰胺(PtBA-b-PNIPAM)嵌段共聚物, 用GPC和 1 H NMR对其结构进行了表征. PtBA-b-PNIPAM在甲苯中水解得到聚丙烯酸-b-聚N-异丙基丙烯酰胺(PAA-b-PNIPAM). 用动态光散射技术对PAA-b-PNIPAM在水溶液中的自组装行为随pH值和温度变化的响应进行了初步研究. 相似文献
57.
表面引发原子转移自由基聚合方法合成Fe3O4/PMMA复合纳米微粒 总被引:7,自引:1,他引:7
采用表面引发原子转移自由基聚合方法合成了核壳结构的磁性高分子纳米微粒. 作为聚合反应引发剂的3-氯丙酸, 首先与油酸修饰的Fe3O4纳米微粒表面的部分油酸置换, 然后在Fe3O4纳米微粒表面引发甲基丙烯酸甲酯聚合, 合成的纳米复合材料用TEM, FTIR, XRD和DSC表征. 磁性测试结果表明, 所制备的磁性高分子纳米微粒仍具有超顺磁性, 但由于聚合物的存在, 其饱和磁化强度降低. 相似文献
58.
Polyelectrolyte multilayer thin films were prepared via the alternate deposition of poly(allylamine hydrochloride) (PAH) and a blend of poly(acrylic acid) (PAA) and poly(styrenesulfonate) (PSS). When the pH of the blend solution was 3.5, the presence of PAA in this solution significantly increased the total film thickness. With only 10 wt % PAA in the blend adsorption solution, a large increase in film thickness was observed (92 nm cf. 18 nm). It was also demonstrated that the total amount of PSS adsorbed was enhanced by the presence of PAA in the blend solution, showing that the blend solution composition influenced that of the multilayer films. Thin films prepared with nanoblended layers also showed improved pH stability, because they exhibited reduced film rearrangement upon exposure to acidic conditions (pH = 2.5). 相似文献
59.
The use of inductively coupled plasma mass spectrometry (ICP-MS) coupled with separation techniques for the purpose of elemental speciation has recently gained a lot of attention. Much of this is due to ever improving separation capabilities of Chromatographic techniques, the high sensitivity of ICP-MS, and the continuing development of better interface techniques. Additionally, there is a growing awareness of the need to monitor various species of an analyte, rather than just total analyte concentrations, due to their often varying natures. For the sake of learning from different elemental speciation approaches, this review brings together some selected types of elemental speciation which have been recently seen in literature. These include separations using various forms of liquid chromatography, such as reversed phase, reversed phase ion pairing, micelle, ion exchange, and size exclusion. Elemental speciation employing gas Chromatographie separations and supercritical fluid separations are discussed as well as elemental speciation using capillary electrophoresis. 相似文献
60.