摘要
建立了微池加压溶剂萃取(μ-PLE)-气相色谱在线联用测定可吸入固体颗粒物(PM10)中多环芳烃的方法和装置.研究了萃取压力在5～20 MPa、萃取温度在50～200℃、萃取时间在2～15 min对μ-PLE萃取效率的影响.实验结果表明:方法的回收率在24.3%～63%之间;对标准样品的检出限为2.2～9.5 μg/L;对实际样品的检出限在0.01～2.03 ng/m3之间;相对标准偏差(RSD)为1.6%～26.4%.通过对萃取池小型化,利用毛细管气相色谱大体积柱内进样技术,实现了两者的在线联用.将萃取液全部转移到气相色谱中,样品利用率达到80%以上,检出灵敏度比现有样品预处理方法提高100倍以上,可以监测大气颗粒中短时间化学变化的有机成分.
A micro pressurized liquid extraction device （μ-PLE） coupled on-line with capillary gas chromatography （CGC） through large volume injection （LVI） was developed and evaluated for the determination of polycyclic aromatic hydrocarbons （PAHs） on PM10 samples. Variables affecting the PLE efficiency such as the pressure, temperature and time of the extraction were studied and optimized in the pressure range of 5 - 20 MPa, temperature range of 50 -200℃ and extraction time of 2 - 15 min, respectively. The recovery of the method was in the range of 24.3% - 63% ; the detection limit for standard sample was 2.2 - 9.5 μg/L, and was 0.01 -2.03 ng/m^3 for real sample, with relative standard deviation between 1.6% and 26.4%. The miniaturization of PLE system and the use of LVI complete transference of the extraction solvent onto 80%, and enhances the detection sensitivity above chemical changes on atmospheric particle matters. technique allows on-line coupling of PLE and CGC. The the CGC increases the utilization of the sample more than 100 times. The method is applicable to monitor short time
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2005年第9期1231-1234,共4页
Chinese Journal of Analytical Chemistry
基金
国家高技术研究发展计划(863计划)资助项目(No.2001AA641040)
