土壤中苯系物的顶空气相色谱_质谱联用测定方法研究.pdfVIP

农业环境科学学报 2010,29(4):812-816 Journal of Agro-Environment Science 土壤中苯系物的顶空气相色谱-质谱联用 测定方法研究 鲁炳闻，韩春媚，周友亚，薛南冬，李发生，谷庆宝 （中国环境科学研究院土壤污染与控制研究室，北京 100012） 摘 要：苯系物是有机化学品泄漏事故中导致土壤污染的主要污染物之一，但我国目前还没建立土壤中苯系物的标准监测方法。 采用顶空气相色谱-质谱联用法（GC-MS）研究了模拟污染土壤中苯系物的测定方法，优化了顶空作为土壤中苯系物预处理方法的 参数，分析了顶空GC-MS 测定的精密度、回收率、检出限和定量限等质量控制参数。结果表明，基质修正液加入量2 mL、顶空平衡 温度70 ℃和顶空平衡时间10 min 为最佳的顶空方法参数；在11~550 μg ·kg-1 的质量浓度范围内，苯系物各组分的浓度与选择离子 峰面积线性相关系数均大于0.99 。采用该方法测定土壤中苯系物的平均加标回收率为89.77%~98.64%，相对标准偏差为0.72%~ 4.64% （n=5）；苯系物的检出限（S/N=3）为0.01~0.21 μg ·kg-1 ，定量限（S/N=10）为0.03~0.71 μg ·kg-1 。 关键词：土壤；苯系物；顶空；GC-MS 中图分类号：X830.2 文献标志码：A 文章编号：1672- 2043(2010)04- 0812- 05 Determination of Benzene and Its Analogues in Soil with Headspace GC-MS LU Bing-wen, HAN Chun-mei, ZHOU You-ya, XUE Nan-dong, LI Fa-sheng, GU Qing-bao （Department of Soil Pollution Control, Chinese Research Academy of Environmental Sciences, Beijing 100012, China） Abstract ：Benzene and its analogues are common organic pollutants in soil as consequence of uncontrolled spills, accidents of organic chemicals. However, standard method for monitoring of benzene and its analogues has not been established in China. Method of determination of benzene and its analogues in soil with headspace GC-MS was studied in this paper. Working parameters for headspace was optimized. Quality control parameters such as precision, recovery of standard, limit of detection and limit of quantification for the process were deter－ mined. Results showed that 2 mL of matrix modifying solution with equilibrium temperature 70 ℃ and time 10 minutes were the best for headspace procedure. The linear scope of the method was 11~550 μg ·kg-1 soil, and the correlation coefficients were higher than 0.99. The av－ erage recovery, accuracy, limit of detection and limit of quantification of this method were in the range of 89.77%~98.64 %, 0.72%~4.64%, 0.01~0.21 μg ·kg-1 and 0.03~0.71 μg ·kg-1 respectively for