GC-MS法同时测定水性涂料中的苯系物和乙二醇醚及其酯类化合物
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摘要
建立了同时测定水性涂料中6种苯系物、5种乙二醇醚及其酯类化合物的GC-MS分析方法,对样品前处理及色谱分析条件进行了优化。样品中加入二乙二醇二甲醚作内标,加入甲醇震荡离心、无水硫酸钠除水,经有机滤膜过滤后供GC-MS测定,采用内标法定量。结果表明,目标物含量在2.0～100 mg·L~(-1)范围内呈良好的线性关系,相关系数大于0.999,方法的检出限为0.13～0.29 mg·L~(-1),样品回收率为在87.4%～108.3%之间,相对标准偏差在0.8%～4.9%之间(n=6)。方法前处理简单、检出限低,准确可靠,满足水性涂料中苯系物和乙二醇醚及其酯类物质的检测需求。
A gas chromatography-mass spectrometry(GC-MS)method was developed for the simultaneous determination of 6 benzene series, 5 glycol ethers and its esters in water-based coatings. Sample preparation and the instruments conditions were optimized. Diethylene glycol dimethyl ether was added as internal standard for quantitative analysis. The coatings were extracted by methanol, dehydrated, filtered and detected. The results showed good linearity in the range of 2.0～100 mg·L~(-1) with the correlation coefficients(R~2) higher than 0.999, the detection limit was 0.13～0.29 mg·L~(-1), the spiked recoveries were 83.1%～112.5% with relative standard deviations of 0.8%～4.9%(n=6). The proposed method is simple, sensitive, and accurate for the simultaneous determination of benzene series compounds and glycol ethers compounds in water-based coatings.
A gas chromatography-mass spectrometry(GC-MS)method was developed for the simultaneous determination of 6 benzene series, 5 glycol ethers and its esters in water-based coatings. Sample preparation and the instruments conditions were optimized. Diethylene glycol dimethyl ether was added as internal standard for quantitative analysis. The coatings were extracted by methanol, dehydrated, filtered and detected. The results showed good linearity in the range of 2.0～100 mg·L~(-1) with the correlation coefficients(R~2) higher than 0.999, the detection limit was 0.13～0.29 mg·L~(-1), the spiked recoveries were 83.1%～112.5% with relative standard deviations of 0.8%～4.9%(n=6). The proposed method is simple, sensitive, and accurate for the simultaneous determination of benzene series compounds and glycol ethers compounds in water-based coatings.
引文
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[7] 张伟亚,李英,刘丽,等.顶空进样气质联用法测定涂料中12种卤代烃和苯系物[J].分析化学,2003,31(2):212-216.
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[9] 周宇艳,程欲晓,陈潜,等.气相色谱-质谱法同时测定水性涂料中的五种乙二醇醚及其酯类化合物[J].环境化学,2013,32(10):1999-2001.
[2] Maldonado G,Delzell E,Tyl R W,et al.Occupational exposure to glycol ethers and human congenital malformations[J].International archives of occupational and environmental health,2003,76(6):405-423.
[3] Andrew F D,Hardin B D.Developmental effects after inhalation exposure of gravid rabbits and rats to ethylene glycol monoethyl ether[J].Environmental health perspectives,1984,57:13-23.
[4] 环境保护部.国家污染物环境健康风险名录——化学第一分册[M].北京:中国环境科学出版社,2009.
[5] 李进颖.我国涂料标准中苯系物和乙二醇醚及其醚酯类溶剂限量的研究[J].涂料技术与文摘,2017,38(12):29-32.
[6] 吴亚虎,黄会芳.涂料及胶粘剂中苯、甲苯、及二甲苯含量的气相色谱测定方法探讨[J].涂料工业,2003,33(6):34-36.
[7] 张伟亚,李英,刘丽,等.顶空进样气质联用法测定涂料中12种卤代烃和苯系物[J].分析化学,2003,31(2):212-216.
[8] 陈会明,王超,王星,等.毛细管气相色谱法检测水性涂料中三种乙二醇醚[J].理化检验(化学分册),2006,42(5):374-376.
[9] 周宇艳,程欲晓,陈潜,等.气相色谱-质谱法同时测定水性涂料中的五种乙二醇醚及其酯类化合物[J].环境化学,2013,32(10):1999-2001.