邻苯二甲酸二异癸酯毛细管柱的制备及其对甲酚二甲酚异构体的分离性能  

Preparation of di-iso-decylphthalate capillary columns and application for cresol and xylenol homologue isomers

作　　者：陈名浪 秦金平[1] 李亚琴[1] 董飞[1] 

机构地区：[1]南京工业大学化学化工学院,江苏南京210009

出　　处：《南京工业大学学报（自然科学版）》2014年第5期42-45,89,共5页Journal of Nanjing Tech University(Natural Science Edition)

摘　　要：采用自制的邻苯二甲酸二异癸酯（DIIDP）毛细管柱对甲酚、二甲酚异构体进行分离和分析.考察多种脱活剂和复配固定液对DIIDP毛细管柱制备的影响,并研究DIIDP含量和柱温对酚类异构体分离性能的影响.结果表明：采用邻苯二甲酸乙二醇聚酯脱活剂成功研制出0.25 mm×30 m×0.2 μm DIIDP色谱柱,在120 ℃时,对甲酚、二甲酚异构体的分离效果较好,每米理论板数为2 800（邻甲酚）,最高使用温度为130℃.复配分析表明：采用SE-54固定液与质量分数20％ DIIDP的二氯甲烷溶液复配制备的毛细管柱分离效果最好,在柱温为130℃时,能将甲酚、二甲酚异构体完全分离,每米理论板数可达3 600以上（邻甲酚）,最高使用温度可达到140～ 150℃。Cresol and xylenol homologue isomers were separated by di-iso-decylphthalate （DIIDP） capillary columns.Several important influence factors were discussed in the preparation of DIIDP capillary columns, including the kind of deactivation reagents and mixed stationary liquid. The effects of the content of DIIDP and the oven tempemture on the separation performance of the phenolic isomers were also investigated.Results showed that the DIIDP chromatographic column of 0. 25 mm× 30 m ×0.2 μm was developed using the reagent of polyethylene glycol phthalate, and the column showed high performance in the separation of cresol and xylenol homologue isomers at the oven temperature of 120 ℃. The number of theoretical plates per meter was 2 800 for o-cresol, and the maximum operation temperature was 130 ℃. Composite analysis showed that with the capillary column prepared by mixed liquid SE-54 with 20% DIIDP dichloromethane solution, cresol and xylenol homologue isomers could be completely separated at 130 ℃ ,the minimum number of theoretical plates per meter was more than 3 600 for o-cresol, and the maximum operation temperature could reach 140-150 ℃.

关 键 词：毛细管色谱柱 邻苯二甲酸二异癸酯 甲酚 二甲酚 异构体 

分 类 号：O657.8[理学—分析化学]