裂解-气相色谱/质谱法定性筛选电子电气产品中六溴环十二烷

建立了热裂解-气相色谱/质谱法快速定性筛选电子电气产品聚合物材料中六溴环十二烷(HBCDD)的方法。聚合物样品经粉碎或剪切后,直接引入热裂解器,以300℃瞬间裂解的方式将HBCDD从聚合物材料中解吸出来,进入气相色谱-质谱联用仪,采用VF-5MS毛细管柱(15 m×0.25 mm×0.1μm)分离,通过保留时间和化合物特征离子定性。优化的实验条件下,HBCDD在200~1500 mg/kg的浓度范围内线性关系良好,相关系数均大于0.99。不同的聚合物基质中,方法的检出限均可达到100 mg/kg。阳性样品采用标准加入法进行半定量分析,相对标准偏差小于20%。本方法简单快速,固体样品直接进样,样品用量少,灵敏度高,能满足日常检测的快速筛选要求。

Determination of Hexabromocyclododecane in the Electrical and Electronic ProductsQualitative Screening by Pyrolyzer-Gas Chromatography-Mass Spectrometry

A qualitative screening method has been developed for the determination of hexabromocyclododecane(HBCDD)in the electrical and electronic products by pyrolyzer-gas chromatography-mass spectrometry(PY-GC/MS).The polymer sample that has been crushed or sheared was directly introduced into the pyrolyzer,HBCDD was resolved from the polymer by instantaneous cracking at 300℃,then was transferred to gas chromatography-mass spectrometry,separated by VF-5 MS capillary column(15 m×0.25 mm×0.1μm),HBCDD was identified based on the retention times and characteristic ions.Under the optimized experimental conditions,the good linear relationship was obtained between values of peak area and mass concentration of HBCDD in the range of 200 to 1500 mg/kg,the correlation coefficient more than 0.99.In different polymers,detectiom limit could reach 100 mg/kg.Positive samples were analyzed semi-quantitatively by standard addition method,and RSD was less than 20%.The method is simple and quick,solid sample of small amount is injected directly,and the sensitivity is high.It can meet the requirements of rapid screening for routine testing.