泡沫六溴环十二烷的测试和替代研究
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摘要
研究建立了测定泡沫中六溴环十二烷的气相色谱质谱(GCMS)方法。样品经丙酮:正己烷(1∶1)混合液超声提取45min后,萃取液通过气相色谱质谱-选择离子监测法进行定量分析。线性相关系数>0.995,平均回收率为95.9%～106%,相对标准偏差(n=6)小于15%。方法简便快速、灵敏度高、定量准确,满足泡沫中六溴环十二烷的检测要求。通过检测后发现部分泡沫不合格,各厂家进行了有效的整改。
A gas chromatography mass spectrometry(GC-MS) method was established for the determination of hexabromocyclododecane in foam. After ultrasonic extraction of the sample by acetone:n-hexane(1∶1) mixture for 45 min, the extract was quantitatively analyzed by gas chromatography-mass spectrometry-selective ion monitoring. The linear correlation coefficient was 0.999, the average recovery was 95.9 %～106 %, and the relative standard deviation(n=6) was less than 15 %. The method is simple, rapid, sensitive and accurate, and meets the detection requirements of hexabromocyclododecane in the foam. After testing, it was found that some of the foams were unqualified, and each manufacturer carried out effective rectification.
A gas chromatography mass spectrometry(GC-MS) method was established for the determination of hexabromocyclododecane in foam. After ultrasonic extraction of the sample by acetone:n-hexane(1∶1) mixture for 45 min, the extract was quantitatively analyzed by gas chromatography-mass spectrometry-selective ion monitoring. The linear correlation coefficient was 0.999, the average recovery was 95.9 %～106 %, and the relative standard deviation(n=6) was less than 15 %. The method is simple, rapid, sensitive and accurate, and meets the detection requirements of hexabromocyclododecane in the foam. After testing, it was found that some of the foams were unqualified, and each manufacturer carried out effective rectification.
引文
[1]阮毅,叶典贤,方正.碳骨架-气相色谱法测定电子电气材料中六溴环十二烷[J].理化检验-化学分册,2015.51(8):1093-1095.
[2]唐志锟,陈强,李丹,等.气象色谱-质谱法测定涂料中的六溴环十二烷[J].理化检验-化学分册,2012.48(7):807-809.
[3]李婷,侯晓东,陈文学,等.超声波萃取技术的研究现状及展望[J].安徽农业科学,2006,34(13):3188-3190.
[2]唐志锟,陈强,李丹,等.气象色谱-质谱法测定涂料中的六溴环十二烷[J].理化检验-化学分册,2012.48(7):807-809.
[3]李婷,侯晓东,陈文学,等.超声波萃取技术的研究现状及展望[J].安徽农业科学,2006,34(13):3188-3190.