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

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.