全蒸发顶空气相色谱-质谱法用于固体体积测定及吸附性能分析  

Full evaporation headspace gas chromatography-mass spectrometry for the volumetric measurement and adsorption performance of irregular solids

作　　者：高元吉 季宝成 赵丽娟[1] GAO Yuanji;JI Baocheng;ZHAO Lijuan(College of Chemistry and Materials Science,Sichuan Nornial University,Chengdu 610068;College of Food and Biological Engineering,Zhengzhou University of Light Industry,Zhengzhou 450001)

机构地区：[1]四川师范大学化学与材料科学学院,成都610068 [2]郑州轻工业大学食品与生物工程学院,郑州450001

出　　处：《分析试验室》2021年第4期390-393,共4页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金项目(51873133,31901767)资助。

摘　　要：结合非固体接触式的全蒸发技术(FET)与顶空气相色谱-质谱联用(HS-GC-MS)技术构建了一种可用于不规则材料的体积分析方法。以苯乙烯和异丙苯为目标分析物,利用气相分子平衡浓度与质谱信号响应值这两个变量之间的线性关系,实现了对多种不规则材料体积的准确测定及其吸附性能分析。实验结果表明:对于以搅拌子为代表的非吸附型材料,全蒸发顶空气相色谱-质谱(FEHS-GC-MS)的响应值不受平衡温度影响,可在不同温度条件下准确计算出其体积;石蜡和石墨烯气凝胶等吸附型不规则材料,可先通过绘制平衡温度-蒸发目标分子吸附曲线研究其吸附性能,然后选取适宜的全脱附温度用于测算其真实体积。该研究为不规则材料的体积测算及其吸附性能研究提供了一种分析策略,可用于新型多孔吸附材料和固相微萃取涂层材料等研究领域。A full evaporation headspace gas chromatography-mass spectrometry(FEHS-GC-MS)combining with full evaporation technique(FET)and headspace sampling techniques was established for novel,rapid,and automatic detecting the volume of irregular solid.The adsorption and desorption characteristics of the solid samples were investigated when the analytes(styrene or cumene)were transferred from solvent phase to gas phase,and finally achieved a dynamic equilibrium.Continuous FEHS-GC-MS method was carried out to investigate the volumetric changes and adsorption performances of irregular solids.The results showed that GCMS peak area values were not affected by equilibration temperature for the non-adsorbent solid like agitators.Therefore,accurately volumetric measurement was obtained for various solid materials at different temperature.In addition,the adsorption performance of the adsorptive irregular materials(such as paraffin and graphene aerogel)was investigated by drawing adsorption curve between the equilibrium temperature and the gaseous target molecule.The appropriate total desorption temperature was selected to calculate the true volume.This method provides a novel,efficient,and convenient strategy for the volumetric change detection for irregular materials,which has great application potential in adsorption of new porous material and coating of solid phase microextraction.

关 键 词：苯乙烯 异丙苯 全蒸发顶空气相色谱质谱法 体积测算 吸附性能 

分 类 号：TS207.5[轻工技术与工程—食品科学] O657.7[轻工技术与工程—食品科学与工程]