Determination of polybrominated biphenyls and polybrominated diphenyl ethers in polymer materials of electronic and electrical products by gas chromatography-mass spectrometry with thermal desorption
YU Shu-yuan1,2, YANG Jun-fan1, SU Dan1, WU Jing-wu1, XIE Tang-tang1, REN Cong*1
1. Shenzhen Customs, Shenzhen 518067, China; 2. Shenzhen Inspection ＆Quarantine Research Institute, Shenzhen 518045, China
Abstract：Polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs) belong to persistent organic pollutants, so it was of great significance to determine and control the contents of PBBs and PBDEs in polymer materials of electronic and electrical products. In traditional methods, the sample should be pretreated before determination, which was cumbersome or relatively large amount of samples were required. After the target compounds were desorbed from the sample by thermal desorption and analyzed by gas chromatography-mass spectrometry (GC-MS), the determination of PBBs and PBDEs in polymer materials of electronic and electrical products by GC-MS with direct solid injection was realized with only mg-level amount of sample required. The thermal desorption conditions such as thermal desorption temperatures, thermal desorption time and heating rate were optimized. The results showed that the linear range was 100-2000mg/kg with correlation coefficient higher than 0.996 under the optimized experimental conditions. The limits of detection were between 5.4mg/kg and 24.8mg/kg, and the limits of quantification were between 18.0mg/kg and 82.6mg/kg. The contents of PBBs and PBDEs in certified reference material of polypropylene (ERM-EC591) were determined for parallel 7 times according to the experimental method. The determination results were basically consistent with the certified values for PBBs and PBDEs when their contents were higher than the limits of quantification. The relative standard deviation (RSD, n=7) was less than 15%. Qualitative and quantitative analysis of PBBs and PBDEs in 20 batches of polymer materials of electronic and electrical products were carried out with the experimental method. The determination results were compared with those obtained by GC-MS with soxhlet extraction in appendix A of standard method of GB/T 26125-2011. The results showed that the contents of all PBBs and partial PBDEs in polymer materials of electronic and electrical products were below the limits of quantification. The relative errors of determination results of other PBDEs with those obtained by standard method were between 3.7% and 15.7%.
余淑媛, 杨俊凡, 苏丹, 吴景武, 谢堂堂, 任聪. 热脱附-气相色谱质谱法测定电子电气产品聚合物材料中多溴联苯和多溴联苯醚[J]. 冶金分析, 2020, 40(3): 25-31.
YU Shu-yuan, YANG Jun-fan, SU Dan, WU Jing-wu, XIE Tang-tang, REN Cong. Determination of polybrominated biphenyls and polybrominated diphenyl ethers in polymer materials of electronic and electrical products by gas chromatography-mass spectrometry with thermal desorption. , 2020, 40(3): 25-31.
AMELIA K,JONAS B,ULRIKA F.Identification of the flame retardant decabromodiphenyl ethane in the environment[J].Environmental Science & Technology,2004,38(12):3247-3253.
[2]
ANDREAS S,HAKAN C,KAJ T,et al.Electronics recycling plant and at other work environments[J].Environmental Science & Technology,2001,35(3):448-454.
[3]
李佐卿,俞雪钧,殷居易,等.电子电气产品中多溴联苯和多溴二苯醚的高效液相色谱/串联质谱法测定[J].分析科学学报,2007,23(4):421-423.LI Zuo-qing,YU Xue-jun,YIN Ju-yi,et al.Determination of polybrominated biphenyls and polybrominated biphenyl ethers in electrical and electronic equipments by liquid chromatography/tandem mass spectrum[J].Journal of Analytical Science,2007,23(4):421-423.
[4]
张瑞,张志辉,刘卓钦,等.高效液相色谱法测定皮革中20种溴代阻燃剂[J].分析试验室,2014,33(1):73-75.ZHANG Rui,ZHANG Zhi-hui,LIU Zhuo-qin,et al.Determination of 20 kinds of brominated flame retardants in leather by HPLC method[J].Chinese Journal of Analysis Laboratory,2014,33(1):73-75.
[5]
王亚伟,张庆华,刘汉霞,等.高分辨气相色谱-高分辨质谱测定活性污泥中的多溴联苯醚[J].色谱,2005,23(5):492-495.WANG Ya-wei,ZHANG Qing-hua,LIU Han-xia,et al.Determination of polybrominated diphenyl ethers in sewage sludge by high resolution gas chromatography coupled with high resolution mass spectrometry[J].Chinese Journal of Chromatography,2005,23(5):492-495.
[6]
Li Q,Loganath A,Chong Y S,et al.Determination and occurrence of polybreminated diphenyl ethers in maternal adipose tissue from inhabi tants of Singapore[J].Chromatography B-analytical Technologies in the Biomedieal and Life Science,2005,819(2):253-257.
[7]
林竹光,张莉莉,孙若男,等.动物肝脏中九种多溴联苯醚残留量的GC-NCI/MS分析[J] .分析试验室,2008,27(7):30-34.LIN Zhu-guang,ZHANG Li-li,SUN Ruo-nan,et al.Determination of nine polybrominated diphenyl ethers residues in animal liver by gas chromatography-negative[J].Chinese Journal of Analysis Laboratory,2008,27(7):30-34.
[8]
孙凤璨,戴尽璇.索氏萃取-GC-ECD法测定电子产品中多溴二苯醚[J].化工时刊,2011,25(1):141-143.SUN Feng-can,DAI Jin-xuan.Soxhlet extraction and GC-ECD for measurement of PBDEs in electronic products[J].Chemical Industry Times,2011,25(1):141-143.
[9]
叶曦雯,牛增元,张清智,等.气相色谱-质谱法测定压敏胶及其制品中的多溴联苯与多溴二苯醚[J].分析测试学报,2013,32(10):1251-1253.YE Xi-wen,NIU Zeng-yuan,ZHANG Qing-zhi,et al.Determination of PBBs and PBDEs in pressure-sensitive adhesive and its products by GC-MS[J].Journal of Instrumental Analysis,2013,32(10):1251-1253.
