热重-流动载气液滴微吸附体系的建立及其应用于卷烟纸的热解产物分析

摘要

将液相微萃取技术用于流动载气条件下热重逸出组分的吸附,自行设计和建立了热重-流动载气液滴微吸附(TG-GFSDMA)联用装置,并结合气相色谱-质谱(GC-MS),建立了可以进行热重逸出组分分析的检测系统.使用该系统并结合划分温度段连续取样法,研究了卷烟纸在主失重区的热失重行为及其热解逸出产物,并考察了热重载气流量对液滴微吸附(SDMA)富集效果的影响.此外,以热解逸出产物中各化合物的相对含量差异,验证了检测系统的可靠性及其应用于热解逸出产物分析的可行性.结果表明:此检测系统在复杂逸出组分分析方面具有明显优势;320～340℃范围内共检测到18种主要热解逸出产物,根据其相对含量计算所得的相对标准偏差(n=5)均小于5%;在100～400 mL/min载气流量范围内,随着载气流量的提高,液滴微吸附可获得更好的吸附效果.%A system of thermogravimetry-gas flow single drop micro-adsorption-gas chromatographymass spectrometry (TG-GFSDMA-GC-MS) was established for the evolved species analysis on pyrolysis of cigarette paper with a continuous sampling method in different temperature ranges. Using this method, the pyrolysis behavior and evolved species from pyrolysis reaction were studied, and the effect of gas flow to adsorption was also discussed. The results indicated that the system could be used for the qualitative and semiquantitative analysis of evolved species from thermogravimetry, and RSD (n=5) calculated from the relative content of 18 pyrolysis products in 320-340 ℃ temperature range were all below 5％. TG-GFSDMA-GC-MS shows obvious advantages in analysis of complex pyrolysis products that conclude furan-2-carbaldehyde, methyl furan-2-carboxylate, allyl butyrate, etc.