Determination of Acrylates in Soil and Sediment by Head-Space Gas Chromatography
摘 要
提出了顶空-气相色谱法测定土壤和沉积物中丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸甲酯、丙烯酸丙酯和丙烯酸丁酯等5种丙烯酸酯类化合物含量的方法。分别选择70 ℃及20 min作为样品在顶空瓶中的平衡温度和平衡时间。用HP-INNOWAX毛细管色谱柱(30 m×0.32 mm,0.32 μm)分离,氢火焰离子化检测器测定。5种丙烯酸酯类化合物在9 min内能完全分离。5种丙烯酸酯类化合物的质量分数在20.0~2 000 μg·kg-1范围内与其峰面积呈线性关系,检出限(3S/N)在2.0~10.0 μg·kg-1之间。方法用于土壤和沉积物样品分析,加标回收率在86.8%~104%之间,测定值的相对标准偏差(n=6)在3.5%~5.4%之间。
Abstract
Five acrylates, including methyl acrylate, ethyl acrylate, methyl methacrylate, propyl acrylate and butyl acrylate in soil and sediments were determined by head-space GC. The temperature and time chosen for equilibration of the sample in the head-space vessel were 70 ℃ and 20 min respectively. HP-INNOWAX capillary chromatographic column (30 m×0.32 mm, 0.32 μm) was used for separation, and hydrogen FID was adopted in the determination. Under the optimum conditions, the 5 compounds were separated within 9 min. Linear relationships between values of peak area and mass concentration of 5 acrylates were obtained in the same range of 20.0-2 000 μg·kg-1, with detection limit (3S/N) in the range of 2.0-10.0 μg·kg-1. The proposed method was applied to the analysis of samples of soil and sediment, giving values of recovery found by standard addition method in the range of 86.8%-104%. Values of RSD′s (n=6) were found in the range of 3.5%-5.4%.
中图分类号 O657.7
所属栏目 工作简报
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收稿日期 2011/12/24
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备注胡文凌(1981-),女,江西九江人,工程师,硕士,主要从事环境监测工作。
引用该论文: HU Wen-ling,PANG Ming,LI Li,ZHANG Jie,YE Zhao-xia,CAO Yan. Determination of Acrylates in Soil and Sediment by Head-Space Gas Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(2): 196~198
胡文凌,庞明,李莉,张杰,叶朝霞,曹艳. 顶空-气相色谱法测定土壤和沉积物中丙烯酸酯类化合物[J]. 理化检验-化学分册, 2013, 49(2): 196~198
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【3】王力,王琳玲,赵天珍,等.超声萃取沉积物中六氯苯的研究[J].分析科学学报, 2006,22(6):663-666.
【4】张晓梅,张竹青,黄文鹏.超声萃取-高效液相色谱法测定土壤中多环芳烃[J].环境科学与管理, 2010,35(7):124-127.
【5】MIELKE H W, WANG G, GONZALES C R, et al . PAH and metal mixtures in new orleans soils and sediments[J] . Science of the Total Environment, 2001,281:217-227.
【6】俞是聃.快速溶剂萃取-气相色谱-质谱联用法测定土壤中多氯联苯Aroclor系列[J].理化检验-化学分册, 2009,45(3):288-292.
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【8】罗庆,孙丽娜.微波辅助萃取气相色谱质谱法测定土壤、底泥及植物样品中的多环麝香[J].分析试验室, 2011,30(4):50-53.
【9】田靖.顶空/气相色谱法测定土壤中挥发性芳烃[J].环境科学与管理, 2007,32(11):125-128.
【10】孙华.土壤中挥发性有机物的顶空制备方法研究[J].干旱环境监测, 2008,22(2):68-72.
【11】王永华,李立人,刘欣,等.顶空气相色谱法测定土壤或底泥中挥发性苯系物[J].中国环境监测, 2011,27(1):17-20.
【12】EPA 5021-1996Volatile organic compounds in soils and other solid matrices using equilibrium headspace analysis[S].
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