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Synthesis of Phenyl-functionalized Mesoporous Material MCM-48 and Its Application in Solid-phase Microextraction

Author: LiChunLan
Tutor: DuXinZhen
School: Northwest Normal University
Course: Analytical Chemistry
Keywords: Mesoporous materials Phenyl functionalized Synthesis Application Solid phase micro extraction
CLC: TB383.4
Type: Master's thesis
Year: 2008
Downloads: 27
Quote: 0
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Abstract


1992 Mobil Corporation researchers first synthesized crystalline silicate / aluminosilicate mesoporous MCM-41 M41S family of mesoporous materials and considered to be the real beginning of Ordered porous materials synthesis. The series of materials including the six-party like (hexagona), MCM-41, cubic (cubic) MCM-48 and layered (lamellar) MCM-50 (Figure 1-1). M41S Series mesoporous material having a high specific surface area, the long-range order and a narrow distribution of the pore structure, high pore volume, as well as an inorganic material or an inorganic base material with a certain degree of mechanical strength and chemical stability and other characteristics, Since the advent of widespread concern. Inorganic / organic composite mesoporous materials in the structure and performance of the many advantages of mesoporous silica and its derivatives, as a new type of inorganic or inorganic / organic composite functional materials in many fields of catalysis, adsorption and separation has broad application prospects. Solid phase micro extraction (SPME) is Pawlisayn proposed in 1990 a set of sample extraction and enrichment in one sample pre-treatment technology. SPME method has the advantages of easy to operate, fast and easy quantitative instruments, together with the analysis with gas chromatography (GC), high performance liquid chromatography (HPLC), capillary electrophoresis (CE) can be widely used in water, soil, air trace amounts of organic and inorganic compounds, determination of environmental samples and blood, urine and other biological samples, as well as food, medicines and other complex samples. Extraction fiber coating of the core parts of the SPME solid-phase micro-extraction technology research, in addition to the commercialization of the polymer coating materials, research and development of the various characteristics of the coating material. This article attempts to phenyl-the C6H5-MCM-48 functionalized the composite mesoporous material used as the SPME fiber coating, made of extraction head and extraction measured in environmental samples benzo [a] pyrene and phthalic dibutyl. This thesis is divided into two parts, a total of five chapters. Chapter One: Summary of the the Mesoporous synthesis and its application in adsorption and separation. Chapter II: solid phase micro-extraction technology and its coating research progress. Chapter III: phenyltrimethoxysilane as a coupling agent, according to the co-hydrolysis polycondensation step synthesis phenyl functionalized mesoporous silica (C6H5-MCM-48), by small angle X-ray diffraction, infrared spectroscopy elemental analysis, differential thermal - weightlessness, nitrogen adsorption - desorption, scanning electron microscopy and titration of composite materials characterization. Chapter: C6H5-MCM-48 mesoporous material as solid phase micro extraction coating materials, preparation of new solid phase micro extraction fiber. By Solid Phase Microextraction Coupled with High Performance Liquid Chromatography (SPME-HPLC), measured in environmental water samples benzo [a] pyrene; such as extraction and desorption time, extraction temperature, stirring speed and ionic strength extraction conditions investigated by changing the extraction efficiency of the coating of the C6H5-MCM-48. Investigated under optimized conditions, the linear range of the method detection limit, precision and recovery. The characteristics of this method reflects the SPME sample pre-treatment process is rapid, sensitive, simple and without solvent. Chapter 5: Introducing a new coating mesoporous material C6H5-MCM-48 as a solid phase micro extraction (SPME) and high performance liquid chromatography (HPLC) combined with the determination of the actual samples phthalate dibutyl (DBP ) methods. Investigated methods optimized SPME conditions such as extraction time, extraction temperature, ionic strength, desorption time reproducibility, linear range and detection limit using the method of analysis of environmental water samples and actual samples obtained satisfaction results.

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