PDF《超声波提取 ￣气相色谱氢火焰测定土壤中六溴环十二烷》

第32 卷第3期2019 年3月环境科学研究Research of Environmental Sciences Vol.

32?No.3 Mar.?2019 收稿日期: 2018~03~15 修订日期: 2018~10~31 作者简介: 王馨蕾(1994~)?女?陕西西安人?846143349@ qq.com. ?责任作者?崔兆杰(1963~)?男?山东龙口人?教授?博士?博导?主要从事环境监测、土壤修复、生命周期评价研究?cuizj@ sdu.edu.cn 基金项目: 鞍钢集团矿业有限公司资助项目(No.2018~科A18) Supported by Projected of Anshan Iron &

Steel Group Mining Co. Ltd.? China (No.2018~科A18) 超声波提取~气相色谱氢火焰测定土壤中六溴环十二烷 王馨蕾? 崔兆杰? 山东大学环境科学与工程学院? 山东 青岛

266000 摘要: HBCD (六溴环十二烷? hexabromocyclododecane)是一种常用的溴代阻燃剂?其对环境和生物体造成的影响已被定性为持 久性有机污染物. 为了建立超声波提取、气相色谱检测土壤中 w(HBCD)的方法?分别对超声波提取 HBCD 条件及气相色谱检测 HBCD 参数进行优化?并对超声波提取法与索氏提取法进行了比较. 结果表明:①最佳超声波提取土壤中 HBCD 条件为以体积比 为1∶1的正己烷:丙酮溶液为提取溶剂?60 ℃ 水浴振荡?超声波提取

50 min. ②气相色谱优化后提取 HBCD 的最佳分离条件为进 样口温度

240 ℃ ?初始温度

90 ℃ ?保留

1 min?升温程序为

90 ℃ 时以

15 ℃ Mmin 升温至

160 ℃ ?保留

2 min?再以

10 ℃ Mmin 升至

220 ℃ ?保留

2 min?最后以

5 ℃ Mmin 升至

280 ℃ ?保留

3 min?分流模式为不分流?以氮气为载气?进样量为

1 μL?FID 检测器温度 为300 ℃ . ③HBCD 在土壤中的平均回收率可达 97? 1%?相对标准偏差为 3? 5%?方法精密度高. ④与索氏提取方法相比?超声波 提取法提取时间短、样品用量少、灵敏度高?并且方法重现性和精密度较好?能更有效地分析土壤中 w(HBCD). 研究显示?场地 土壤中 w(HBCD)平均值为 0?

757 mgMkg?相对标准偏差为 4? 22%(小于 5%)?超声波提取及气相色谱检测土壤中 HBCD 的方法准 确度高、重现性好?对分析土壤中 HBCD 更加简便快捷. 关键词: 六溴环十二烷? 气相色谱? 超声波提取? 土壤 中图分类号: X833 文章编号: 1001~6929(2019)03~0493~07 文献标志码: A DOI: 10? 13198Mj? issn? 1001~6929? 2018? 11?

10 Determination of Hexabromocyclododecane in Soil by an Ultrasonic Extraction~ Gas Chromatography with FID Method WANG Xinlei? CUI Zhaojie? School of Environmental Science and Engineering? Shandong University? Qingdao 266000? China Abstract: Hexabromocyclododecane (HBCD)? a commonly used brominated flame retardant? has been identified as a persistent organic pollutant (POP) due to its effects on the environment and organisms. In order to establish a method for the determination of HBCD in soils by ultrasonic extraction and gas chromatography ( GC)? the conditions of ultrasonic extraction and gas chromatography analysis were optimized. The ultrasonic extraction was compared with soxhlet extraction. The experimental results indicated that: (1) The optimum extraction conditions were

25 mL of mixed solvents of hexane and acetone (1 ∶

1 VMV)?

60 ℃ ? and

50 min extraction time. (2) The optimum inlet temperature for the gas chromatography was

240 ℃ . The initial temperature of the column was kept at

90 ℃ for

1 min? increased to

160 ℃ at

15 ℃ Mmin for

2 min? and then raised to

220 ℃ at

10 ℃ Mmin for

2 min. Finally? the temperature was raised to