含铁二氧化硅涂层固相微萃取-GC/MS法测定水中的有机磷阻燃剂  

Determination of organophosphorus flame retardants in water by solid phase microextraction-GC/MS method with iron-containing silica coating

作　　者：赵佳平 王俊霞[1] 刘婷婷 张占恩[1,2] ZHAO Jia-ping;WANG Jun-xia;LIU Ting-ting;ZHANG Zhan-en(School of Environmental Science and Engineering,Suzhou University of Science and Technology,Suzhou 215009,China;Collaborative Innovation Center of Water Treatment Technology and Material,Suzhou University of Science and Technology,Suzhou 215009,China)

机构地区：[1]苏州科技大学环境科学与工程学院,江苏苏州215009 [2]苏州科技大学水处理技术与材料协同创新中心,江苏苏州215009

出　　处：《现代化工》2021年第9期235-240,共6页Modern Chemical Industry

基　　金：国家“十三五”水专项课题(2017ZX07205-02);江苏省环境科学与工程重点实验室项目(Zd1805);苏州市科研计划项目(SNG2018050)。

摘　　要：制备了含铁的二氧化硅材料,并以涂敷式自制了固相微萃取纤维,建立了顶空固相微萃取-气质联用技术测定环境水样中5种典型有机磷阻燃剂的检测方法。对材料进行了SEM-EDS、XRD、氮气吸附脱附以及热重分析表征,结果表明,材料热稳定性好,有丰富的孔道结构。考察了萃取温度、时间、pH、盐质量分数的影响,最佳分析条件为:萃取温度为80℃,萃取时间为30 min,pH为3,盐质量分数为30%;在最佳条件下,5种有机磷阻燃剂的检出限为2.1~32.6 ng/L。应用于太湖水和某污水处理厂出水中磷酸酯阻燃剂的检测,获得了较高的加标回收率(69.4%~113.7%)和精密度(5.3%~10.7%)。Iron-containing silica material is prepared,and it is made into solid phase microextraction fiber through coating route. The method to determine 5 typical types of organophosphorus flame retardant in environmental water samples is established based on headspace solid phase microextraction/gas chromatography-mass spectrometry. The prepared material is characterized by SEM-EDS,XRD,nitrogen adsorption and desorption,and thermogravimetric analysis.Characterization results prove that the material has good thermal stability and abundant pore structure.Effects of extraction temperature,time,pH,and salt concentration are investigated. The best conditions are obtained as follows:extraction temperature is at 80℃,extraction time is 30 min,pH is 3,and salt concentration is 30%. Under the optimal conditions,the detection limits of the five types of organophosphorus flame retardants are in the range of 2. 1-32. 6 ng·L-1.As it is applied to the detection of phosphate ester flame retardant in Taihu Lake water and the effluent of a sewage treatment plant,high recovery rate( 69. 4%-113. 7%) and precision( 5. 3%-10. 7%) are obtained.

关 键 词：固相微萃取 二氧化硅 有机磷阻燃剂 气相色谱质谱 

分 类 号：TH3[机械工程—机械制造及自动化]