【作者】 田锐；

【导师】 侯经国； 高锦章；

【作者基本信息】 西北师范大学 ， 分析化学， 2005， 硕士

【摘要】 1992年Mobil公司的科学家对M41S（MCM-41、MCM-48、MCM-50）系列硅基（silica-based）介孔分子筛的合成揭开了分子筛科学的新纪元。作为一种新型功能材料,介孔材料由于其具有较大的比表面积和孔容、长程有序的孔道结构、良好的扩散性能以及机械和热稳定性等优点,自问世以来就受到广泛关注,尤其被广泛应用于催化、吸附和分离等领域。随着研究的深入,介孔材料的应用已扩大到光电材料、新型电池、敏感元件、药物载体、色谱分离和分子生物工程等领域。同时,各种含杂原子、非硅基、有机官能化介孔材料的合成更加拓宽了其应用范围。 固相微萃取（Solid-phase microextraction, SPME）是由加拿大渥太华大学的Pawliszyn教授在1990年提出的一种新型的集萃取、浓缩、解吸于一体的样品前处理技术。由于该技术具有操作简单、价廉实用等特点而备受分析工作者和仪器制造商的重视。SPME技术在与气相色谱（GC）、高效液相色谱（HPLC）、毛细管电泳（CE）等分析仪器联用后可广泛应用于水、土壤、空气等环境样品和血、尿等生物样品,以及食品、药物等各种复杂样品中痕量有机、无机物的测定。萃取纤维涂层是SPME的核心部位,除了常用的商品化的聚合物涂层材料外,对各种特性涂层材料的开发研究是目前固相微萃取技术研究的热点。 本论文由两大部分组成,第一部分为综述部分,第二部分为实验部分。 第一章:综述了介孔材料的合成及应用。 第二章:综述了近几年固相微萃取技术及其涂层研究进展。 第三章:以二甲基二氯硅烷为偶联剂修饰了介孔分子筛MCM-41,将有机官能团引到介孔分子筛MCM-41表面,制备了一种无机-有机复合材料CH₃-MCM-41,用小角XRD、SEM、元素分析和IR技术对其进行了表征。 第四章:以辛基三甲氧基硅烷和十八烷基三氯硅烷为硅烷化试剂采用后处理接枝技术对介孔分子筛MCM-41的表面进行了烷基化修饰,合成了无机-有机复合材料C₈-MCM-41和C₁₈-MCM-41并进行了表征。 第五章:将C₁₈-MCM-41介孔分子筛用做固相微萃取涂层材料,制备了新型的固相微萃取纤维。通过固相微萃取与高效液相色谱联用（SPME-HPLC）,测定了环境水体中的菲,对萃取时间、萃取温度、离子强度、解吸时间等SPME条件进行了优化,建立了SPME-HPLC测定环境水体中菲的新方法。更多还原

【Abstract】 Ordered mesoporous materials have received a great deal of attention, as a novel mesoporous material, M41S, was firstly reported by researchers in the Mobil laboratory in the early 1990s, because of their potential applications in catalysis, separation technology, nanoscience, and biomaterials. Compared with microporous materials, mesoporous materials not only have larger surface area (up to 1500 m2/g) and thicker wall between pores, uniform pore size distribution (-1.5-40 nm) and huge pore volume, but also they have excellently mechanical and chemical stability. They were widely used as catalysts, sorbents and separation materials in the past decade. Up to now a great variety of functionalized and morphologic momesoporous materials have been developed in order to obtain higher selectivity and special action sites.Solid-phase microextraction (SPME) as a new solvent-free extraction technique in sample preparation appeared in the early 1990s. Because of its advantages of simplicity, rapid extraction and easy quantification, SPME was successfully applied to extracting and concentrating for various analytes in environmental samples (gas, liquid, solid), foodstuff, biological samples and materia medica. SPME could be easily coupled with the apparatus, such as gas chromatography (GC) and high performance liquid chromatography (HPLC). Fiber with coating is the most important part of SPME, the selectivity and the extraction efficiency of the fiber depend considerably on the coating materials. Up to date many experimental coatings have been prepared and investigated for a wide range of applications. The coating materals that were universally used in SPME are various polymer-based coatings, such as polydimethylsiloxane (PDMS) and polyacrylate (PA), which were coated on fused silica fibers. However, specialized materials have been also developed for special demand in SPME. In this dissertation, our effort is to synthesize new functionalized mesoporous materials and use as coating materials in SPME for analysis of environmental samples by high-performance liquid chromatography coupling with SPME technique.The dissertation consists of six parts:更多还原