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  

Determination of butyl acrylate and 2-ethylhexyl acrylate in sewage by gas chromatography-mass spectrometry

作　　者：吴志鹏 唐毅 桑柳波 邵峙玮 Wu Zhipeng;Tang Yi;Sang Liubo;Shao Zhiwei(New Materials Research Institute of CASCHEM(ChongQing)Co.,Ltd.,Chongqing400000,China)

机构地区：[1]中科广化(重庆)新材料研究院有限公司,重庆400000

出　　处：《化学分析计量》2021年第6期21-25,共5页Chemical Analysis And Meterage

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)。

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,0.25μm)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0.03μg/L和0.05μg/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。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,0.25μm),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 0.03μg/L and 0.05μg/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 

分 类 号：O657.7[理学—分析化学]