溶胶-凝胶固相微萃取涂层的制备及特性  

Preparation and Characteristics of New Coating for Solid Phase Microextraction

作　　者：丁有毅 温泉[2] 闫秀媛[2] 隋丽丽[2] 

机构地区：[1]齐齐哈尔质量技术监督检验检测中心,黑龙江齐齐哈尔161006 [2]齐齐哈尔大学化学化工学院,黑龙江齐齐哈尔161006

出　　处：《化工时刊》2008年第11期42-44,共3页Chemical Industry Times

基　　金：黑龙江省教育厅科学技术研究项目(编号11531410)

摘　　要：采用溶胶-凝胶法,将含高化学活性的四乙氧基硅烷（前驱体）与羟基硅油混和,以三氟乙酸为催化剂,经水解、缩合化学反应,形成溶胶体系,在石英纤维表面经陈化胶粒间聚合形成凝胶。将键合于石英表面上的凝胶作为固相微萃取涂层。采用FTIR红外光谱法表征了溶胶-凝胶的三维网络结构。应用溶胶-凝胶法制备的固相微萃取涂层热稳定性好,不易脱落。采用HS-SPME-GC技术萃取分析了水中的氯苯、苯、甲苯,以色谱峰高对浓度作外标曲线,在0.1~20 mg/L范围内,苯、甲苯、氯苯的线性相关系数分别为0.991 2、0.978 2、0.974 4,最低检测限分别为0.06、0.04、0.10 mg/L。实验结果表明自制的硅橡胶涂层对芳香化合物具有良好的吸附特性。In the paper, tetraethoxy-silicane（precursor） containing high chemical activity and hydroxy silicone oil was mixed, trifluoroacetic acid as catalyst, Sol-system which was getted by the reaction of hydrolysising and condensation formed gel through aging and polymerizing among particles at quartz fiber surface. The three-dimensional network structure was characterized by Fourier transform infrared spectroscopy. The solid-phase microextraction coating was prepared by the gel binding in quartz fiber surface. The solid-phase microextraction coating was prepared by sol-gel technology was thermally stable and hardly cracking-off. The coating was used to detect chlorobenzene, benzene and Toluene by using HS-SPME-GC united technology. Equlibrium temperature and extraction time were chosen. In 0. l mg/L -20mg/L, the linear relationships beteen the contents of compents and their peak heights is good. The correlation coefficients ofbenzene and Toluene,chlorobenzene were 0.991 2,0.978 2,0.974 4 respectively. The detection limits of benzene,Toluene and chlorobenzenewere 0.06 mg/L,0.04 mg/L,0.10 mg/L respectively. The experiment results indicated that the complex coating has particular property for extracting chloroarenes.

关 键 词：溶胶-凝胶 固相微萃取涂层 气相色谱 应用 

分 类 号：O658.2[理学—分析化学]