物理化学学报 >> 2013, Vol. 29 >> Issue (12): 2481-2497.doi: 10.3866/PKU.WHXB201310152

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对固体圆二色光谱测试方法的再认识——兼谈“浓度效应”

章慧1,3, 颜建新1, 吴舒婷2, 李丹1, 万仕刚1, 丁雷1, 林丽榕1   

  1. 1 厦门大学化学化工学院化学系, 福建厦门 361005;
    2 福州大学化学化工学院化学系, 福州 350108;
    3 中国科学院福建物质结构研究所, 结构化学国家重点实验室, 福州 350002
  • 收稿日期:2013-07-19 修回日期:2013-10-14 发布日期:2013-11-28
  • 通讯作者: 章慧, 吴舒婷 E-mail:huizhang@xmu.edu.cn;shutingwu@fzu.edu.cn
  • 基金资助:

    国家自然科学基金(21273175, 21271150, 21001026)和中国科学院福建物质结构研究所结构化学国家重点实验室基金(20110006, 20130008)资助项目

Further Understanding on the Measurement Methods for Solid-State Circular Dichroism Spectroscopy——Discussion on Concentration Effects

ZHANG Hui1,3, YAN Jian-Xin1, WU Shu-Ting2, LI Dan1, WAN Shi-Gang1, DING Lei1, LIN Li-Rong1   

  1. 1 Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, Fujian Province, P. R. China;
    2 Department of Chemistry, College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou 350108, P. R. China;
    3 State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Struture of Matter, Chinese Academy of Sciences, Fuzhou 350002, P. R. China
  • Received:2013-07-19 Revised:2013-10-14 Published:2013-11-28
  • Contact: ZHANG Hui, WU Shu-Ting E-mail:huizhang@xmu.edu.cn;shutingwu@fzu.edu.cn
  • Supported by:

    The project was supported by the National Natural Science Foundation of China (21273175, 21271150, 21001026) and State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences (20110006, 20130008).

摘要:

对近期发展的固体圆二色(CD)光谱测试方法进行了概述、评价和比较, 着重探讨了“浓度效应”的存在使固体CD光谱失真的原因. 通过对本课题组和其他作者已报道的四种化合物的固体CD谱再测试的反思, 强调了依手性化合物的手性光谱学性质不同, 根据浓度梯度实验选择其合适测试浓度的必要性. 对固有手性的阻转异构化合物(S)-1,1'-联二萘酚(S-BINOL)进行了成膜法固体CD谱浓度梯度测试, 发现所得固体薄膜CD谱中也存在着“浓度效应”

关键词: 固体手性光谱, 圆二色, 测试方法, 浓度效应, 阻转异构, 镜面对称性破缺

Abstract:

In this paper, the recent developments in measurement methods of solid-state circular dichroism (CD) spectroscopy were summarized and discussed, especially the effects of concentration on solid-state CD spectral distortions. By reinspection and introspection of the solid-state CD spectra of four reported compounds, concentration gradient measurements were proved to be necessary for appropriate concentrations, which are greatly related to the chiroptical properties. The thin film solid-state CD measurements of the inherently chiral atropisomer (S)-1,1'-bi-2-naphthol (S-BINOL) were carried out with concentration gradient measurements. Using this film-state technique for the first time, the results show some subtle correlations between the CD curves and the special concentrations.

Key words: Solid-state chiroptical spectroscopy, Circular dichroism, Method of measurement, Concentration effect, Atropisomerism, Mirror symmetry breaking

MSC2000: 

  • O641