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《化学分析计量》 2021年第06期
DOI:10.3969/j.issn.1008-6145.2021.06.005
气相色谱-质谱法测定污水中丙烯酸丁酯和丙烯酸-2-乙基己酯
吴志鹏,唐毅,桑柳波,邵峙玮
中科广化(重庆)新材料研究院有限公司,重庆 400000 
Determination of butyl acrylate and 2-ethylhexyl acrylate in sewage by gas chromatography-mass spectrometry
Wu Zhipeng, Tang Yi, Sang Liubo, Shao Zhiwei
New Materials Research Institute of CASCHEM(ChongQing) Co., Ltd., Chongqing 400000, China 
摘要:建立气相色谱-质谱仪测定农村污水中丙烯酸丁酯和丙烯酸-2-乙基己酯的方法。取200 mL污水样品置于250 mL分液漏斗中,加入5 g氯化钠和10 mL乙酸乙酯,置于全自动旋转振荡器上充分振荡萃取10 min,静置分层后,弃去下层水相,将上层有机相除水后转移至10 mL容量瓶中,用乙酸乙酯准确定容至标线,稍作振荡,静置后经有机相滤膜过滤,待测。提取液用SH-Rtx-5MS色谱柱(30 m×0.25 mm,0.25 μm)分离,选择离子监测/全扫描(SIM/SCAN)模式,气相色谱-质谱法测定。丙烯酸丁酯和丙烯酸-2-乙基己酯在0.002~1.0 mg/L范围内与其色谱峰面积具有良好的线性关系,当样品取样量为200 mL时,丙烯酸丁酯和丙烯酸-2-乙基己酯的检出限分别为0.03 最/L和0.05 最/L。丙烯酸丁酯和丙烯酸-2-乙基己酯的加标回收率分别为92.3%~101.1%、93.2%~109.9%,测定结果的相对标准偏差分别为0.8%~1.5%、0.9%~2.9%(n=6)。该方法可用于农村污水中丙烯酸丁酯和丙烯酸-2-乙基己酯的测定。 
Abstract:A gas chromatography-mass spectrometer method was established for determination of butyl acrylate and 2-ethylhexyl acrylate in rural sewage. 200 mL of sample, 5 g sodium chloride and 10 mL ethyl acetate were added into a 250 mL separatory funnel, then the separatory funnel was place on a fully automatic rotary shaker to fully shake and extract for 10 min. After standing for stratification, discard the lower aqueous phase, transfer the upper organic phase to a 10 mL volumetric flask after dewatering, accurately dilute to the mark with ethyl acetate, shake it aside, and filter through the organic phase filter for testing. The extract was separated by SH-Rtx-5MS chromatographic column (30 m×0.25 mm, 0.25 μm), and determined by gas chromatographic mass spectrometry in SIM/SCAN mode. The two acrylates had good linear relationship with the chromatographic peak area in the range of 0.002-1.0 mg/L. When the sample volume was 200 mL, the detection limits of butyl acrylate and 2-ethylhexyl acrylate were 0.03 最/L and 0.05 最/L, respectively. The recovery rates of butyl acrylate and 2-ethylhexyl acrylate were 92.3%-101.1% and 93.2%-109.9%, respectively. The relative standard deviations of the measurement results were 0.8%-1.5% and 0.9%-2.9%(n=6) for butyl acrylate and 2-ethylhexyl acrylate, respectively. The method can be used for the determination of butyl acrylate and 2-ethylhexyl acrylate in rural sewage. 
关键词:液液萃取;气相色谱-质谱法;污水;丙烯酸丁酯;丙烯酸-2-乙基己酯 
Keywords:liquid-liquid extraction; gas chromatography-mass spectrometry; sewage; butyl acrylate; 2-ethylhexyl acrylate 
基金:重庆北碚区技术创新与应用示范产业类项目(编号2019–31) 
本文引用格式:
吴志鹏,唐毅,桑柳波,等.气相色谱-质谱法测定污水中丙烯酸丁酯和丙烯酸-2-乙基己酯[J].化学分析计量,2021,3030(6):21.
Wu Zhipeng,Tang Yi,Sang Liubo,et al. Determination of butyl acrylate and 2-ethylhexyl acrylate in sewage by gas chromatography-mass spectrometry[J]. Chemical Analysis and Meterage,2021,30(6):21. 

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