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作 者:胡文凌[1] 庞明[1] 李莉[1] 张杰[1] 叶朝霞[1] 曹艳[1]
出 处:《理化检验(化学分册)》2013年第2期196-198,201,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
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,0.32μm)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20.0~2000μg·kg^(-1)范围内与其峰面积呈线性关系,检出限(3S/N)在2.0~10.0μg·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。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 rain respectively. HP-INNOWAX capillary chromatographic column (30 m×0. 32mm, 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%.
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