加速溶剂萃取法与索氏提取法对废线路板中二噁英测定的影响

引用本文: 蔡璐, 赵文杰, 周全法. 加速溶剂萃取法与索氏提取法对废线路板中二噁英测定的影响[J]. 分析化学, 2017, 45(5): 687-692. doi: 10.11895/j.issn.0253-3820.160767 shu

Citation: CAI Lu, ZHAO Wen-Jie, ZHOU Quan-Fa. Determination of Dioxin in Waste Printed Circuit Boards by Accelerated Solvent Extraction and Soxhelt Extraction[J]. Chinese Journal of Analytical Chemistry, 2017, 45(5): 687-692. doi: 10.11895/j.issn.0253-3820.160767 shu

加速溶剂萃取法与索氏提取法对废线路板中二噁英测定的影响

江苏理工学院江苏省电子废弃物资源循环利用重点实验室, 常州 213001
基金项目:
本文系国家科技支撑计划项目（No. 2014BAC03B06）、联合国开发计划署全球环境基金项目（No. 20141201CN）、江苏省重点研发计划（No.BE2016657）和江苏省普通高校研究生科研创新计划项目（No. 20820111516）资助

摘要: 将经过多级破碎分选所得的废线路板粉末过60目筛，以2 mol/L HCl溶液、超纯水洗涤，并用丙酮脱水。将预处理后的滤渣、滤纸填入萃取池，或者用新滤纸包裹后置于索氏提取管内，添加5 μL内标物，分别用加速溶剂萃取法（ASE）或索氏提取（SE）法进行萃取，依次采用多层硅胶柱和活性炭柱对萃取提取物进行净化、洗脱，得到二噁英测试样品。用同位素稀释-高分辨气相色谱-质谱联用仪分析样品中二噁英的含量。考察两种提取方法及不同氯代数对15种¹³C-2，3，7，8-PCDD/Fs回收率的影响，比较两种方法的准确度和精密度。结果表明，ASE和SE对15种¹³C-2，3，7，8-PCDD/Fs的回收率分别为54.3%~113.0%和28.3%~77.7%，实测废线路板中二噁英毒性当量（Toxic equivalent quangtity，TEQ）分别为0.075 ng TEQ/kg和0.266 ng TEQ/kg。在方法精密度允许范围内，ASE相对具有简单快速、溶剂用量少和准确的优势。

关键词:

English

Determination of Dioxin in Waste Printed Circuit Boards by Accelerated Solvent Extraction and Soxhelt Extraction

Jiangsu Province Key Laboratory of E-Waste Recycling, Jiangsu University of Technology, Changzhou 213001, China
Received Date: 18 October 2016
Revised Date: 12 January 2017
Fund Project:
This work was supported by the National Science-technology Support Plan Projects (No.2014BAC03B06), the UNDP Global Environment Facility (No. 20141201CN), Jiangsu Province Key Research and Development Plam (No. BE2016657) and the Graduate Student Scientific Research Innovation Projects in Jiangsu Province University (No. 20820111516)

Abstract: Waste printed circuit boards(W-PCBs) were multiple smashed and separated, then passed through a 60-mesh screen, treated with hydrochloric acid (2 mol/L), ultrapure water and dehydrated with acetone successively. The filter residue and filter paper were filled into the extraction pool, or inserted into Soxhlet Extraction tube parceled with new filter paper. After addition of 5 μL of internal standard substance, the filter residue above was respectively extracted by Soxhlet Extraction (SE) method or Accelerated Solvent Extraction (ASE) method, cleaned with multi-layer silica gel column and activated-charcoal column to obtained the dioxins samples. The samples were analyzed by isotope dilution high resolution gas chromatography-high resolution mass spectrometry (HRGC-HRMS). The effects of SE and ASE method and number of chlorines atoms on recovery of 15 kinds of ¹³C-2,3,7,8 PCDD/Fs were investigated, and the accuracy and precision of the two extraction methods were compared. The results show that, the recovery of 15 kinds of ¹³C-2,3,7,8 PCDD/Fs using ASE method is 54.3%-113.0%, and that of SE is 28.3%-77.7%, and the Toxic Equivalent Quangtity (TEQ) in W-PCBs is 0.075 ng/kg (TEQ) and 0.266 ng/kg (TEQ) using ASE and SE method respectively. Under the premise that accuracy and precision meet with the international standard, ASE is simple, rapid, solvent-free and accurate.

Key words:

1. [1]
  1 LI Hui-Ru, YU Li-Ping, ZHANG Su-Kun, REN Man, SHENG Guo-Ying, FU Jia-Mo, PENG Ping-An. Chinese J. Anal. Chem., 2008, 36(2):150-156 李会茹, 余莉萍, 张素坤, 任曼, 盛国英, 傅家谟, 彭平安. 分析化学, 2008, 36(2):150-156
2. [2]
  Rimayi C, Chimuka L, Odusanya D, Boer J D, Weiss J. Chemosphere, 2015, 145:314-21
3. [3]
  Duan H B, Li J H, Liu Y C, Norimasa Y, Jiang W. Environ. Sci. Technol., 2011, 45(15):6322-6328
4. [4]
  XU Peng-Jun, TAO Bu, LI Nan, ZHENG Sen, ZHAO Hu, FAN Shuang, ZHOU Zhi-Guang, REN Yue, QI Li, CHEN Ji-Ping. Chinese J. Anal. Chem., 2015, 43(3):356-365 许鹏军, 陶晡, 李楠, 郑森, 赵虎, 范爽, 周志广, 任玥, 齐丽, 陈吉平. 分析化学, 2015, 43(3):356-365
5. [5]
  Guéguen F, Stille P, Millet M. Environ. Sci. Pollut. Res. Int., 2013, 20(6):3852-3862
6. [6]
  Dias-Ferreira C, Kirkelund G M, Jensen P E. Chemosphere, 2016, 148:380-387
7. [7]
  Shin E S, Kim J, Choi S D, Kang Y W, Chang Y S. Chemosphere, 2016, 146:419-425
8. [8]
  Planche C, Ratel J, Mercier F, Blineta P, Debrauwerb L, Engel E. J. Chromatogr. A, 2015, 1392:74-81
9. [9]
  LI Xiang, ZHANG Yao, SUN Yi-Zhi, ZHONG Wei-Ke, QIU Yue-Ming, CHEN Yan-Chang, WANG Da-Ning. Chinese J. Chromatogr., 2006, 24(4):347-350 李翔, 张垚, 孙毅之, 仲维科, 邱月明, 陈彦长, 王大宁. 色谱, 2006, 24(4):347-350
10. [10]
  MA Fei-Pan, ZHANG Su-Kun, ZHAO Bao-Wei, REN Ming-Zhong, XU Jie, QING Xian, ZHANG Man-Wen. Environmental Chemistry, 2014, 33(2):243-247 马飞攀, 张素坤, 赵保卫, 任明忠, 徐洁, 青宪, 张漫雯. 环境化学, 2014, 33(2):243-247
11. [11]
  Method 1613B. Tetra-through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS. US EPA-1997
12. [12]
  ZHAO Shi-Yan, CUI Zhao-Jie. Environ. Protec. Chem. Ind., 2006, 26(6):518-521 赵士燕, 崔兆杰. 化工环保, 2006, 26(6):518-521
13. [13]
  ZHANG Yun, SU Jin, JIN Cheng-Long. Shanghai Journal of Preventive Medicine, 2006, 18(8):368-372 张昀, 苏瑾, 金成龙. 上海预防医学杂志, 2006, 18(8):368-372
14. [14]
  Nie Z Q, Die Q Q, Yang Y F, Tang Z W, Wang G Q, Huang Q F. Environ. Sci. Pollut. Res., 2014, 21(13):7863-7875
15. [15]
  Berit B, Uta R. K, Norbert T. Environ. Sci. Pollut. Res., 2015, 22(24):19887-19895
16. [16]
  Zhang P, Ge L K, Zhou C G, Yao Z W. Chin. J. Oceanol. Limnol., 2011, 29(5):1103-1112
17. [17]
  MA Jun-Wei, WANG Zhen-Zhen, YANG Zhi-Feng, NIE Yong-Feng,BAI Qing-Zhong. Techniques and Equipment for Environmental Pollution Control., 2005, 6(7):63-66 马俊伟, 王真真, 杨志峰, 聂永丰, 白庆中. 环境污染治理技术与设备, 2005, 6(7):63-66
18. [18]
  GAO Dan, LIU Jin-Song, ZHU Guo-Hua, GONG Hong-Ping, ZHOU Xin,WANG Ling, MO Wei-Min, LI Mu-Fei. Chinese J. Anal. Chem., 2013, 41(12):1862-1868 高丹, 刘劲松, 朱国华, 巩宏平, 周欣, 王玲, 莫卫民, 李霂菲. 分析化学, 2013, 41(12):1862-1868
19. [19]
  YU Bin-Bin, FANG Cheng, RAO Qin-Quan, CHEN Tao, MOU Yi-Jun, WU Zu-Cheng. Chinese J. Anal. Chem., 2011, 39(6):833-838 余彬彬, 方铖, 饶钦全, 陈涛, 牟义军, 吴祖成. 分析化学, 2011, 39(6):833-838
20. [20]
  HJ 77.3-2008, Solid Waste Determination of Polychlorinated Dibenzo-p-Dioxins(PCDDs)and Polychlorinated Dibenzofurans(PCDFs)Isotope Dilution HRGC-HRMS. National Standards of the People's Republic of China 固体废物二噁英类的测定同位素稀释高分辨气相色谱-高分辨质谱法. 中华人民共和国国家标准.HJ 77.3-2008
21. [21]
  DU Bing, LIU Ai-Min, HUANG Ye-Ru. Chinese Journal of Chromatography, 2004, 32(9):867-970 杜兵, 刘爱民, 黄业茹. 色谱, 2004, 32(9):867-970
22. [22]
  GB 5085.6-2007, Identification Standards for Hazardous Waste-Identification for Extraction Toxicity. National Environmental Protection Standard of the People's Republic of China 危险废物鉴别标准/毒性物质含量鉴别. 中华人民共和国国家环境保护标准. GB 5085.6-2007

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沈阳化工大学材料科学与工程学院沈阳 110142

加速溶剂萃取法与索氏提取法对废线路板中二噁英测定的影响

English

Determination of Dioxin in Waste Printed Circuit Boards by Accelerated Solvent Extraction and Soxhelt Extraction

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加速溶剂萃取法与索氏提取法对废线路板中二噁英测定的影响

English

Determination of Dioxin in Waste Printed Circuit Boards by Accelerated Solvent Extraction and Soxhelt Extraction

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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