气相色谱-质谱法测定塑料中四溴双酚A
GC-MS Determination of Tetrabromobisphenol A in Plastics
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摘要: 提出了气相色谱-质谱法测定塑料中四溴双酚A含量的方法。样品经乙酸乙酯超声提取20 min后,氮气吹干。用甲苯5.0 mL溶解残渣,经乙酸酐衍生化后,所得衍生产物过DB-5MS色谱柱分离,电子轰击离子源质谱检测。四溴双酚A的质量浓度在0.1~100 mg·L-1范围内与其峰面积呈线性关系。以ABS和PS塑料样品为基体,进行加标回收试验,回收率在分别为97.0%和94.2%,相对标准偏差(n=5)小于6.5%。Abstract: GC-MS was applied to the determination of tetrabromobisphenol A in plastics. The sample was extracted with ethyl acetate for 20 min, and concentrated to dryness by N2-blowing. The residue was dissolved with 5.0 mL of methylbenzene, and derivatized with acetic anhydride. The derivatized products were separated on DB-5MS column and EI source was used in MS. Linear relationship between values of peak area and mass concentration of tetrabromobisphenol A was kept in the range of 0.1-100 mg·L-1. Tests for recovery were made by standard addition method with 2 samples of plastics (ABS and PS) as matrixes; values of recovery found were 97.0% for ABS and 94.2% for PS with RSD′s (n=5) less than 6.5%.