气相色谱法测定电子产品中十溴联苯醚
GC Determination of Decabromodiphenyl Ether in Electronic Products
摘 要
提出了气相色谱法测定电子产品中十溴联苯醚的方法.样品先后用甲苯超声提取和浓硫酸提取,所得有机相经硅胶层析柱净化和二氯甲烷洗脱后,以PCB-103为内标物,采用气相色谱法,用电子捕获检测器检测.十溴联苯醚与内标峰面积的比值对十溴联苯醚与内标物质量浓度比值在0.01~10.0 mg·L-1范围内呈线性,检出限(3S/N)为8.0 μg·kg-1.方法用于电视机塑料外壳中十溴联苯醚的测定,相对标准偏差(n=5)为2.2%~8.9%,回收率在92.1%~95.3%之间.
十溴联苯醚
电子产品
GC-ECD
Decabromodiphenyl ether
Electronic products
Abstract
Contents of decabromodiphenyl ether (BDE-209) in electronic products was determined by GC.The sample was extracted with toluene and con.H2SO4 in succession.The organic phase was purified and concentrated on silica-gel chromatographic column and eluted with dichloromethane.The dluate was used for GC-ECD analysis after adding PCB-103 as internal standard.Linear relationship between values of peak area ratios of the BDE-209 standard to internal standard and mass concentration of BDE-209 was obtained in the range of 0.01-10.0 mg·L-1,with detection limit (3S/N) of 8.0 μg·kg-1.The proposed method was applied to the analysis of plastic shells of TV-sets,giving values of RSD′s (n=5) in the range of 2.2%-8.9% and recovery in the range of 92.1%-95.3%.
中图分类号 O657.7
所属栏目 工作简报
基金项目 国家基础科学人才培养基金(J0630429)
收稿日期 2009/1/7
修改稿日期
网络出版日期
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备注涂逢樟(1977-),男,福建长汀人,讲师,硕士,主要从事毛细管电泳、色质联用的研究.
引用该论文: TU Feng-zhang,LIN Zhu-guang,YAO Hui-mei,LI Xiao-bo,PENG Shu-nü. GC Determination of Decabromodiphenyl Ether in Electronic Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(5): 493～496
涂逢樟,林竹光,姚辉梅,李小波,彭淑女. 气相色谱法测定电子产品中十溴联苯醚[J]. 理化检验－化学分册, 2010, 46(5): 493～496
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参考文献
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【14】VETTER W A.GC/ECNI-MS method for the identification of lipophilic anthropogenic and natural brominated compounds in marine samples chromatographic and ionization properties of polybrominated diphenyl ethers using GC-High Resolution MS with metastable atom bombardment and electron impact ionization[J].Anal Chem,2001,73(20):495l-4957．
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【3】李英明,江桂斌,王亚,等.电子垃圾拆解地大气中二噁英、多氯联苯、多溴联苯醚的污染水平及相分配规律[J].科学通报,2008,53(2):165-171．
【4】POLO M,GOMEZ-NOYA G,QUINTANA J B.Development of a solid-phase microextzaction gas chromatography/tandem mass spectrometry method for polybrominated diphenyl ethers and polybrominated biphenyls in water samples[J].Anal Chem,2004,76(4):1054-1062．
【5】SJODIN A,JONES R S,LAPEZA C R.Semiautomated high-throughput extraction and cleanup method for the measurement of polybrominated diphenyl ethers,pdybrominated biphenyls and polyehlorinated biphenyls in human serum[J].Anal Chem,2004,76(7):1921-1927．
【6】宋晟.ROHS指令中多溴联苯、多溴联苯醚的前处理研究[J].计量与测试技术,2009,36(3):28-29．
【7】薛秋红,牛增元,李艳秋,等.GC/MS法测定电子电气塑料件中的限用含溴阻燃剂[J].工程塑料应用,2006,34(7):50-53．
【8】罗峰.气相色谱-质谱测定塑胶中多溴联苯和多溴联苯醚[J].光谱实验室,2008,25(1):23-27．
【9】许骅,方能虎,卫碧文,等.ABS塑料中阻燃剂多溴联苯醚的检测方法[J].理化检验-化学分册,2009,45(1):63-65．
【10】王丽琴,蒋京鑫,柯桢.气相色谱-质谱联用仪测定电子产品中多溴联苯和多溴联苯醚[J].分析仪器,2009,2:21-24．
【11】邵玉婉,邵超英,张琢.气相色谱法测试纺织品中多溴联苯阻燃剂[J].印染,2008,19:30-34．
【12】王成云,杨左军,张伟亚.微波辅助萃取-高效液相色谱法测定塑料中的溴系阻燃剂[J].塑料助剂,2006,56(2):39-43．
【13】王成云,杨左军,张伟亚.塑料中溴系阻燃剂的高效液相色谱法测定[J].深圳职业技术学院学报,2006(1):31-36．
【14】VETTER W A.GC/ECNI-MS method for the identification of lipophilic anthropogenic and natural brominated compounds in marine samples chromatographic and ionization properties of polybrominated diphenyl ethers using GC-High Resolution MS with metastable atom bombardment and electron impact ionization[J].Anal Chem,2001,73(20):495l-4957．
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