碳骨架-气相色谱法测定电子电气材料中六溴环十二烷
GC Determination of Hexabromocyclododecane in Electronic and Electrical Materials Based on Carbon Skeleton
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摘要: 提出了碳骨架-气相色谱法测定电子电气材料中六溴环十二烷的方法.样品经二氯甲烷-丙酮(1+2)混合液超声提取30 min后用正己烷进行溶剂置换,在催化反应衬管中进行钯催化氢化反应.用HP-5MS毛细管色谱柱分离,氢火焰离子化检测器检测.六溴环十二烷的质量浓度在1.25~80.0 mg·L-1范围内与其峰面积呈线性关系,方法的测定下限(10S/N)为10 mg·kg-1.加标回收率在78.8%~106%之间,测定值的相对标准偏差(n=8)为2.1%~5.6%之间.Abstract: A method of GC for the determination of hexabromocyclododecane in electronic and electrical materials based on carbon skeleton was proposed.The sample was ultrasonically extracted with the mixture of dichloromethane-acetone (1+2) for 30 min,and then the solvent was displaced with n-hexane.Catalytic hydrogenation reaction with palladium was conducted on the catalytic liners.The analyte was separated on HP-5MS capillary column and detected by FID.Linear relationship between values of peak area and mass concentration of hexabromocyclododecane was obtained in the range of 1.25-80.0 mg·L-1,with detection limit (10S/N) of 10 mg·kg-1.Values of recovery found by standard addition method were in the range of 78.8%-106%,and values of RSD′s (n=8) in the range of 2.1%-5.6%.