气相色谱-质谱法测定聚氨酯泡沫中3种阻燃剂  

GC-MS Determination of 3 Flame Retardants in Polyurethane Foams

作　　者：陶琳[1] 田野 刘胜[1] 王乐[1] 王辉[1] 许宏民[1] 

机构地区：[1]淄博出入境检验检疫局,淄博255000 [2]张店疾病预防控制中心,淄博255000

出　　处：《理化检验（化学分册）》2015年第11期1520-1523,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家认监委制标项目(2012B413);山东出入境检验检疫局科技计划项目(SK201245)

摘　　要：提出了气相色谱-质谱法测定聚氨酯泡沫中的三（1,3-二氯异丙基）磷酸酯、三（2-氯乙基）磷酸酯和三（2-氯丙基）磷酸酯等3种阻燃剂含量的方法。聚氨酯泡沫样品用丙酮进行索氏抽提,在气相色谱分离中用HP-5MS毛细管柱为固定相,在质谱分析中采用选择离子监测模式。3种阻燃剂在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限（3S/N）在0.4~1.5mg·kg-1之间,测定下限（10S/N）在1.3~5.0mg·kg-1之间。以空白样品为基体进行加标回收试验,所得回收率在84.2%~93.6%之间,测定值的相对标准偏差（n=6）在0.62%~3.3%之间。A method of GC-MS for the determination of 3flame retardants,i.e.tris（1,3-dichloro-2-propyl）phosphate,tris（2-chloroethyl）phosphate and tris（1-chloro-2-propyl）phosphate in polyurethane foams was proposed.The sample of polyurethane foams was extracted by Soxhlet method with acetone.The HP-5MS capillary column was used for GC separation and the selected ion monitoring mode was adopted in MS determination.Linear relationships between values of peak area and mass concentration of the 3flame retardants were kept in definite ranges,with detection limits（3S/N）in the range of 0.4-1.5mg·kg-1 and lower limits of determination（10S/N）in the range of 1.3-5.0mg·kg-1.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 84.2%-93.6%,with RSD′s（n=6）in the range of0.62%-3.3%.

关 键 词：气相色谱-质谱法 聚氨酯泡沫 阻燃剂 

分 类 号：O657.63[理学—分析化学]