柱前衍生-气相色谱-电子捕获法同时检测水体中的9种全氟羧酸

发布时间：2018-01-07 20:26

本文关键词：柱前衍生-气相色谱-电子捕获法同时检测水体中的9种全氟羧酸　出处：《分析化学》2017年02期 　论文类型：期刊论文

【摘要】：建立了柱前衍生-气相色谱-电子捕获(GC-ECD)法同时测定水中PFBA、PFPeA、PFHxA、PFHpA,PFOA,PFNA,PFDA,PFUnA及PFDoA等(全称见正文)9种全氟羧酸(Perfluorinated carboxylic acids,PFCAs)。使用2,4-二氟苯胺(2,4-Difluoroaniline,2,4-DFA)为衍生剂,N,N'-二环己基碳二亚胺(N,N'-Dicyclohexylcarbodiimide,DCC)为脱水剂,与PFCAs形成酰胺衍生产物,衍生产物通过TR-5毛细管色谱柱分离,并以ECD检测器进行检测。对全氟羧酸衍生化过程中2,4-DFA和DCC用量、衍生反应溶剂、反应温度、反应时间等条件进行了优化,得出最佳衍生化条件。结果表明,在最优实验条件下,9种PFCAs衍生产物的线性相关系数0.99,检出限为0.62~1.38μg/L,相对标准偏差RSD为1.3%~7.5%。应用本方法对城市污水中全氟类羧酸进行了分析,城市污水中存在以PFPeA、PFHpA和PFOA为主的痕量PFCAs化合物,实际样品的加标回收率在84.4%~120.9%之间。本方法稳定、可靠、成本低,能够满足水样中多种全氟羧酸的同时检测的要求,可为水体中全氟化合物的污染评价提供技术支持。
[Abstract]:A precolumn derivation-gas chromatography-electron capture spectrometry (GC-ECD) method was developed for the simultaneous determination of PFHxAX (PFHpAN) PFHpAn (PFNAA) and PFDA in water by gas chromatography-electron capture spectrometry (GC-ECD). PFUnA and PFDoA et al. (see perfluorinated carboxylic acidsof 9 perfluorinated carboxylic acidsn, PFCs, etc.). 4- difluoroaniline 2- difluoroaniline 24-DFA) was used as a derivation of N ~ (2 +) -dicyclohexyl carbodiimide (N). Na-Dicyclohexylcarbodiimide (DCCs) was used as dehydrating agent to form amide derivatives with PFCAs. The derivatives were separated by TR-5 capillary column and detected by ECD detector. The amount of 24-DFA and DCC, the solvent and reaction temperature in the process of perfluorocarboxylic acid derivatization were determined. The reaction time and other conditions were optimized and the optimum derivatization conditions were obtained. The results showed that the linear correlation coefficient of the nine PFCAs derivatives was 0.99 under the optimal experimental conditions. The detection limit was 0.62 ~ 1.38 渭 g 路L ~ (-1) and the relative standard deviation (RSD) was 1.3 ~ 7.5. The perfluorocarboxylic acid in municipal sewage was analyzed by this method. There are trace PFCAs compounds mainly PFPeAn PFHpA and PFOA in municipal sewage. The recoveries of the actual samples are between 84.4% and 120.9%. The method is stable. It can meet the requirements of simultaneous detection of various perfluorocarboxylic acids in water samples and provide technical support for the pollution assessment of perfluorocarbons in water.
【作者单位】：浙江万里学院生物与环境学院;湖南大学环境科学与工程学院;湖南大学环境生物与控制教育部重点实验室;
【基金】：国家自然科学基金(No.51408551) 浙江省公益技术应用研究计划项目(Nos.2016C33037,2015C33012,2017C33023) 宁波市自然科学基金(Nos.2016A610232,2015A610253) 浙江省重中之重学科自设课题项目(No.ZS2016005)资助~~
【分类号】：X832;O657.71
【正文快照】： 1引言全氟化合物(Perfluorochemicals,PFCs)是一系列人工合成的、与碳原子相连的氢原子全部被氟原子取代的有机化合物,因为结构中含有大量C-F键使得它能在环境中长期稳定地存在[1,2]。PFCs具有良好的化学稳定性、热稳定性、表面活性及既疏水又疏油的特性,被广泛应用于纸张、

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