基于PDMS的NMR中色谱技术的分离性能研究

doi:10.11938/cjmr20150312

波谱学杂志 ›› 2015, Vol. 32 ›› Issue (3): 511-517.doi: 10.11938/cjmr20150312

基于PDMS的NMR中色谱技术的分离性能研究

吴瑞¹，柏正武^1*，杨盈²，黄少华^2*

1. 武汉工程大学化学与环境工程学院，湖北武汉 430073；2. 中国科学院青岛生物能源与过程研究所，生物基材料重点实验室，山东青岛 266101

收稿日期:2014-07-15 修回日期:2015-07-20 出版日期:2015-09-05 发布日期:2015-09-05
作者简介:吴瑞(1990-)，男，湖北荆门人，硕士研究生，主要从事有机合成分析工作. *通讯联系人：柏正武，电话：027-87194980, E-mail: zhengwu_bai@yahoo.com；黄少华，电话：0532-80662660, E-mail: huangsh@qibebt.ac.cn
基金资助:
国家自然科学基金资助项目(21105108)

Evaluation of Separation Performance of Polydimethylsiloxane-Matrixed Chromatography by NMR

WU Rui¹，BAI Zheng-wu^1*，YANG Ying²，HUANG Shao-hua^2*

1. School of Chemical and Environmental Engineering, Wuhan Institute of Technology, Wuhan 430073, China; 2. Key Laboratory of Biobased-materials, Qingdao Institute of Bioenergy and Bioprocess Technology, Chinese Academy of Sciences, Qingdao 266101, China

Received:2014-07-15 Revised:2015-07-20 Online:2015-09-05 Published:2015-09-05
About author:*Corresponding author: BAI Zheng-wu, Tel: +86-027-87194980, E-mail: zhengwu_bai@yahoo.com; HUANG Shao-hua, Tel: +86-0532-80662660, E-mail: huangsh@qibebt.ac.cn.
Supported by:
国家自然科学基金资助项目(21105108)

摘要/Abstract

摘要：

以聚二甲基硅氧烷(polydimethylsiloxane，PDMS)作为NMR中色谱技术的虚拟“固定相”，利用高分辨液体NMR中的DOSY技术考察其对正戊烷、1-溴戊烷和1,5-二溴戊烷这3种烷烃的分离性能．结果显示，在没有添加PDMS时，上述3种组分的扩散系数较接近，不能被分离；但当检测体系中含有PDMS时，3种组分的扩散系数相差较大，因而能被很好地分离．此外，还研究了样品温度和溶液粘度对分离性能的影响，其影响的趋势为：升高样品温度能改善混合物的分离；而增加溶液粘度则不利于混合物的分离．

关键词: 聚二甲基硅氧烷, 虚拟“固定相”, NMR中色谱技术, DOSY, 混合物分离

Abstract:

Polydimethylsiloxane (PDMS) has been used as the virtual “stationary phase” (VSP) for chromatographic NMR. Its separation capability towards halogenated compounds was investigated. Diffusion coefficients of n-pentane, 1-bromopentane and 1,5-dibromopentane contained in a mixture were measured with high-resolution liquid-state diffusion-ordered NMR spectroscopy (DOSY). In the absence of PDMS, these diffusion coefficients were close, and as a result, the three components could not be separated. In contrast, the diffusion coefficients were markedly different from each other in the presence of PDMS, leading to excellent separation. In addition, the effects of sample temperature and solution viscosity on separation performance were also investigated. It was observed that separation performance improved as sample temperature rose; and reduced as solution viscosity increased.

Key words: polydimethylsiloxane, virtual stationary phase, chromatography NMR, DOSY, separation

中图分类号:

O482.53

吴瑞1，柏正武1*，杨盈2，黄少华2*. 基于PDMS的NMR中色谱技术的分离性能研究[J]. 波谱学杂志, 2015, 32(3): 511-517.

WU Rui1，BAI Zheng-wu1*，YANG Ying2，HUANG Shao-hua2*. Evaluation of Separation Performance of Polydimethylsiloxane-Matrixed Chromatography by NMR[J]. Chinese Journal of Magnetic Resonance, 2015, 32(3): 511-517.

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基于PDMS的NMR中色谱技术的分离性能研究

Evaluation of Separation Performance of Polydimethylsiloxane-Matrixed Chromatography by NMR

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