作者：陈广银¹, 蔡灏兢¹, 朱奕¹, 夏飞², 张晨杰³

作者单位：1. 昆山市环境监测站, 江苏 昆山 215316;
2. 江苏新锐环境监测有限公司, 江苏 张家港 215618;
3. 昆山经济技术开发区安全生产监督管理和环境保护局, 江苏 昆山 215300

关键词：土壤;硝基苯类化合物;气相色谱;超声提取;离心法

摘要：

针对土壤中的硝基苯类化合物测定前处理复杂、设备要求高、损失率高的特点，以及气相色谱法在测试过程中土壤基质复杂、干扰峰面积难以准确定量等问题，研究采用丙酮和正己烷超声提取土壤中的15种硝基苯类化合物，将提取液离心后直接进样测定，并用峰高定量。结果表明：以石英砂为基质的硝基苯及邻、间、对硝基甲苯的检出限为5.7~9.4 g/kg；其他11种硝基苯类化合物检出限为0.2~1.8 g/kg，相对标准偏差0.2%~4.4%。在土壤加标量为40，100，500 g/kg时，硝基苯的加标回收率较低，为61.3%~86.9%；相同浓度的邻、间、对硝基甲苯回收率为78.2%~118%；在土壤加标量为4，10，50 g/kg时，其他11种硝基苯类化合物加标回收率在88.9%~119%之间，相对标准偏差为2.1%~8.3%，平均值为5.2%。该方法前处理过程简单，操作简便、检出限低，经实际样品及加标回收测试，能满足土壤中硝基苯类化合物的监测要求。

An improved ultrasonic extraction-gas chromatography for determination of fifteen nitrobenzene compounds in soils

CHEN Guangyin¹, CAI Haojing¹, ZHU Yi¹, XIA Fei², ZHANG Chenjie³

1. Kunshan Environmental Monitoring Station, Kunshan 215316, China;
2. Jiangsu Xinrui Environmental Monitoring Co., Ltd., Zhangjiagang 215618, China;
3. Supervision and Administration of Safety Production and Environmental Protection Bureau of Kunshan Economic and Technological Development Zone, Kunshan 215300, China

Abstract: In order to solve problems such as complex pretreatment, high equipment requirements and high loss rate appearing when determining nitrobenzene compounds in soils and complex soils matrix and difficult accurate quantification of interference peak area of gas chromatography when testing actual samples, acetone and normal hexane ultrasound are adopted in the research to extract the 15 kinds of nitrobenzene compounds in soils, and the extracting solution is directly determined after being centrifuged and quantified by peak height. The results show that the detection limits of nitrobenzene with matrix being quartz sand and o-, m-, p-nitrotoluene are 5.7-9.4 μg/kg, and the detection limit of other eleven nitrobenzene compounds is 0.2-1.8 μg/kg with relative standard deviation being 0.2%-4.4%. When the soils addition is 40, 100 and 500 μg/kg, the addition recovery rate of nitrobenzene is relatively low(61.3%-86.9%), and the recovery rate of o-, m-, p-nitrotoluene with same concentration is 78.2%-118%. When the soils addition is 4,10 and 50 μg/kg, the recovery rate of the other 11 kinds of nitrobenzene compounds is between 88.9%-119% with the relative standard deviation being 2.1%-8.3% and the average value being 5.2%. The method simplifies the pretreatment process with features including easy operation and low detection limit, which meets the monitoring requirements for nitrobenzene compounds in soils based on actual sample and addition recovery test.

Keywords: soils;nitrobenzene compounds;gas chromatography;ultrasonic extraction;centrifugation

2018, 44(4): 48-52  收稿日期: 2018-01-18;收到修改稿日期: 2018-03-15

基金项目: 

作者简介: 陈广银(1982-),男,安徽颍上县人,工程师,硕士,研究方向为有机物监测与评价。

参考文献

[1] 魏复盛,齐文启,华秀,等. 水和废水监测分析方法指南:中册[M]. 北京:中国环境科学出版社,2003:251-254.
[2] 张蕾,徐镜波. 硝基芳烃对虹鳉鱼的毒性[J]. 生态环境,2004,13(1):31-33.
[3] 张永娟,刘琳,池帛洋,等. 土壤环境中硝基苯的微波萃取-气相色谱法检测技术的研究[J]. 环境科学与管理,2010,35(4):138-140.
[4] 孙壮,李承. 超声提取气相色谱法测定土壤中硝基苯类化合物[J]. 环境科学与技术,2016,39(1):207-209.
[5] 邓延慧,何忠,齐静娴,等. 顶空气相色谱法快速测定土壤中苯、苯胺和硝基苯[J]. 环境监测管理与技术,2009,21(1):22-24.
[6] 孔晔,曹喆. 采用安捷伦5977B GC-MS测定土壤中硝基苯类化合物含量[J]. 环境化学,2017,36(5):1166-1170.
[7] 李皎洁,赵晓松. 硝基苯在土壤中的吸附特征及影响因素[J]. 吉林农业大学学报,2010,32(2):181-185.
[8] 万大娟,李顺义,舒月红,等. 土壤和沉积物中1,2,4-三氯苯的超声波提取[J]. 中山大学学报:自然科学版,2005, 44(3):102-104.
[9] 环境监测分析方法标准制修订技术导则:HJ 168-2010[S]. 北京:中国环境出版社,2010.
[10] ZHANG G J, ZHOU X, ZANG X H, et al. Analysis of nitrobenzene compounds in water and soil samples by graphene composite-based solid-phase micro-extraction coupled with gas chromatography-mass spectrometry[J]. Chinese Chemical Letters,2014,25(11):1449-1454.
[11] 土壤环境监测技术规范:HJ/T 166-2004[S]. 北京:中国环境出版社,2004.