固相微萃取论文：固相微萃取 整体柱 苯系物

固相微萃取：固相微萃取 整体柱 苯系物 固相微萃取论文:固相微萃取 整体柱 苯系物 【中文摘要】固相微萃取(SPME)是一种新型的样品预处理技术, 由于具有操作简单、选择性高、样品量小、无需萃取溶剂等优点近些 年来在分析监测中得到了飞速发展。整体柱由于具有制备简单, 渗透性好、流动相和样品消耗少、环境污染小,易与其他检测方法联 用以及面积大等优点在固相微萃取领域中得到了越来越广泛的应 用。本文以甲基丙烯酸碳酰十八酯(SMA)为功能单体,乙叉二甲基丙烯 酸酯(EDMA)为交联剂,1.4-丁二醇和异戊醇为二元致孔剂,偶氮二异 丁腈(AIBN)作为引发剂,通过原位热引发聚合分别制备了内径为100 μm和530μm的不加硅球和530μm加硅球SMA-co-EDMA整体柱,分 别作为微萃取柱用于样品的浓缩和进样,对萃取条件进行优化后考察 了三种类型微萃取柱的富集倍率。实验表明加入硅球的大内径微萃取 柱的富集倍率明显高于其他两种类型微萃取柱,用该530μm加硅球 微萃取柱浓缩后进样分析,测得该方法对苯,甲苯和丁苯的检出限分 别为3.71μg/L,1.64μg/L,2.52μg/L(相当于噪音信号标准偏差的 3倍),因此该方法可以满足对样品溶液中痕量苯系物的测定。 【英文摘要】Solid-phase microextraction (SPME) as a new sample pretreatment technology have been developed rapidly in recent years since it possesses several attractive features including simple operation, small sample volume, solventless extraction, and high sensitivity. Monolithic column have been used widely in solid phase microextraction fields because of the advantages of simple preparation, good permeability, high spicific surface characteristics, low mobile phase and sample consumption, little pollution, easy integration with other detectors.In this study, two different diameter specifications of monolithic column with 100μm and 530μm was prepared by in-situ free radical polymerization of stearyl methacrylate (SMA) with ethylene glycol dimethacrylate (EDMA) using the porogens composing of iso-amyl alcohol and 1,4-butanediol in the presence of the initiator AIBN.One was entrapped with silica microparticles , and the other without. The prepared monolithic columns were used as the extraction column for sample of enrichment and sample introductin to micro-HPLC. The extraction conditions were optimized experimentally in detail. and the enrichment factors of the microextraction columns were determined under the optimal conditions . It was demonstrated that the obtained enrichment factor using the silica-particle-entrapped microextraction column of larger diameter was obviously higher than using the columns with no entrapped silica particles and the columns of smaller inner diameters. When the silica-particle-entrapped microextraction column of larger diameter was used for sample enrichment and injection to micro-HPLC, the detection limits (equivalent to noise signal standard deviation of 3 times) were determined to be 3.71μg/L, 1.64μg/L and 2.52μg/L for benzene, toluene, and butylbenzene, respectively. The method presented in this study has a good potential to be applied for the determination of trace benzenes in waters. 【关键词】固相微萃取 整体柱 苯系物 采买全文】 1.3.9.9.38.8.4.8 1.3.8.1.13.7.2.1 同时提供论文写作一对一辅导和论文发表服务.保过包发. 【说明】本文仅为中国学术文献总库合作提供，无涉版权。作者如有异议请与总库或学校联系。 【英文关键词】solid-phase microextraction Monolithic column Benzenes in content 【目录】三种C_(18)毛细管整体微萃取柱的应用 摘要 4-5 Abstract 5 1 绪论 8-13 1.1 固相微萃取在 色谱分析中的研究进展 8-10 1.1.1 固相微萃取的基本原理 8-9 1.1.2 固相微萃取萃取涂层的研究进展 9 1.1.3 固相微萃取与其它分析仪器的联用 9-10 1.2 固相微萃取在分 析应用中的现状 10-11 1.3 整体柱在固相微萃取领域中的发 展 11-13 1.3.1 整体柱的特点及应用 11-12 1.3.2 整 体柱在固相微萃取中的研究概况 12-13 2 固相微萃取整体柱 的制备 13-18 2.1 引言 13-14 2.2 整体柱的制备 14-18 2.2.1 实验部分 14-16 2.2.2 结果与讨论 16-18 2.2.3 小结 18 3 三种固相微萃取柱富集倍率的 考察 18-32 3.1 引言 18 3.2 100 μm 内径甲基丙烯酸 碳酰十八酯整体微萃取柱 18-22 3.2.1 引言 18 3.2.2 实验部分 18-20 3.2.3 结果与讨论 20-22 3.3 530 μm 内径甲基丙烯酸碳酰十八酯整体微萃取柱 22-27 3.3.1 引言 22 3.3.2 实验部分 22-23 3.3.3 结果与讨论 23-27 3.4 530 μm 内径加硅球甲基丙烯酸碳酰十八酯整体微萃取柱 27-32 3.4.1 引言 27 3.4.2 实验部分 27-28 3.4.3 结果与讨论 28-32 3.5 小结 32 4 毛细管固相微萃取-液相色谱分析 32-37 4.1 引言 32-33 4.2 实验部分 33-34 4.2.1 仪器 33 4.2.2 试剂与材料 33 4.2.3 毛细管色谱柱制备 33-34 4.2.4.溶液配制 34 4.3 结果与讨论 34-37 4.3.1 直接进样分离分析 34-35 4.3.2 用微萃取柱进样分离分析 35-36 4.3.3 方法评价 36-37 5 结论与展望 37-38 参考文献 38-49 攻读硕士学位期间发表学术论文情况 49-50 致谢 50