研制了一种热解析装置,并与气相色谱或气相色谱-质谱联用,定性定量分析了大气可吸入颗粒物中的半挥发性有机物。装置为直热式加热,升温速率快;直接安装在色谱进样器上方,无需冷阱聚焦。将热解析装置与气相色谱联用,优化了样品承载体材质、热解析条件和进样模式,并用于16种多环芳烃和9种正构烷烃的检测。结果表明,热解析-气相色谱方法对多环芳烃和正构烷烃的检出限分别为0.014~0.093 ng和0.016~0.026 ng,线性相关系数大于0.9975;用于3个城市PM10中的痕量多环芳烃和正构烷烃的定量测定,回收率分别在95%~135%(多环芳烃)和95%~115%(正构烷烃)之间。将热解析装置与气相色谱-质谱联用,比较了3个城市7种粒径分布的PMx(x=10,5,2,1,0.5,0.25,0.1)中的多环芳烃和正构烷烃,结果表明,不同粒径颗粒物均含有正构烷烃和PAHs,但含量相差很大。
A thermal desorption ( TD) device was developed and coupled to gas chromatography ( GC) or gas chromatography-mass spectrometry ( GC-MS ) for the qualitative and quantitative analysis of semi-volatile organic compounds on atmospheric particulate matters ( PM ) . The TD was operated by direct heating and placed on the GC injector, leading to high heating rate and easy transfer of analytes to GC without focusing of analytes by cold trap. For establishing the TD-GC method, the materials used for supporting PM samples, temperature and time of thermal desorption, and types of sample injection were investigated for detection of sixteen polycyclic aromatic hydrocarbons ( PAHs) and nine n-alkanes. The limits of detection of the proposed TD-GC method were in the range of 0. 014-0. 093 ng for PAHs, and 0. 016-0. 026 ng for n-alkanes, respectively, with the correlation coefficients of correlation above 0. 9975. The TD-GC method was applied to the determination of trace PAHs and n-alkanes on PM10 samples from three cities. The recoveries were in the range of 95%-135% ( PAHs) and 95%-115% ( n-alkanes) , respectively. Finally, the TD was coupled to GC-MS for comparison of the contents of PAHs and n-alkanes on PMx with different particulate size ( x=10 , 5, 2, 1, 0. 5, 0. 25, 0. 1).