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羧基膦酸改性氧化锆固定相的制备及其色谱性能
引用本文:姚礼峰,靳素荣,王志花,冯钰锜,达世禄.羧基膦酸改性氧化锆固定相的制备及其色谱性能[J].武汉大学学报(理学版),2005,51(6):659-662.
作者姓名:姚礼峰  靳素荣  王志花  冯钰锜  达世禄
作者单位:1. 武汉大学,化学与分子科学学院,湖北,武汉,430072;武汉理工大学,理学院,湖北,武汉,430070
2. 武汉理工大学,理学院,湖北,武汉,430070
3. 武汉大学,化学与分子科学学院,湖北,武汉,430072
基金项目:国家自然科学基金资助项目(20275029)
摘    要:用十二胺-N乙酸-N亚甲基膦酸(DAPA)改性氧化锆制备了一种新的锆基质色谱固定相(DAPAZ),研究发现,DAPA在氧化锆表面有两种结合方式:红外光谱中1611cm^-1处的特征吸收表明羧基主要与胺基形成偶极离子,以羧酸根离子形式存在,大部分的DAPA分子通过膦酸基团与氧化锆结合;而与钼酸的显色反应则表明有少量DAPA以羧居与氧化锆结合,另外,对固定相的屏蔽效应、碱性条件(pH9.5)下的稳定性等色谱性能的研究也证实这两种吸附方式同时存在,但以膦酸基结合为主。

关 键 词:氧化锆  色谱固定相  十二胺-N乙酸-N-亚甲基膦酸
文章编号:1671-8836(2005)06-0659-04
修稿时间:2005年1月17日

Preparation and Chromatographic Properties of the Dodecylamine N-Acetic Acid-N-Methylenephosphonic Acid Modified Zirconia Stationary Phase
YAO Li-feng,JIN Su-rong,WANG Zhi-hua,FENG Yu-qi,DA Shi-lu.Preparation and Chromatographic Properties of the Dodecylamine N-Acetic Acid-N-Methylenephosphonic Acid Modified Zirconia Stationary Phase[J].JOurnal of Wuhan University:Natural Science Edition,2005,51(6):659-662.
Authors:YAO Li-feng  JIN Su-rong  WANG Zhi-hua  FENG Yu-qi  DA Shi-lu
Institution:YAO Li-feng ~
Abstract:A new zirconia-based stationary phase(DAPAZ) was prepared by modified zirconia with dodecylamine-N-acetic acid-N-methylenephosphonic acid(DAPA).The adsorption mode of DAPA on zirconia was studied in detail.The broad peak at 1 611 cm~(-1) in the FTIR spectra of DAPAZ indicated that the dissociated carboxylic group formed zwitterion with amine group of DAPA,and that most of the DAPA was adsorbed on zirconia with phosphonic group.However,the results of coloration reaction of DAPAZ with ammonium molybdate indicated that some DAPA were adsorbed on zirconia with carboxyl group.These adsorption modes were also supported by the chromatographic behaves and the stability test of the stationary phase at pH 9.5.
Keywords:zirconia  stationary phase  dodecylamine-N-acetic acid-N-methylenephosphonic acid
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