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作 者:薛希妹[1] 薛秋红[2] 刘心同[2] 单宝田[1] 牛增元[2]
机构地区:[1]中国海洋大学化学化工学院,山东青岛266100 [2]山东出入境检验检疫局,山东青岛266000
出 处:《分析测试学报》2011年第5期522-526,共5页Journal of Instrumental Analysis
基 金:2008年山东省自然科技基金资助项目(Y2008B19)
摘 要:建立了溶剂型涂料中16种有害物质(甲醇、卤代烃、苯系物和游离二异氰酸酯)的GC-MS同时检测方法,研究了乙酸乙酯、正己烷、四氢呋喃和乙腈对各有害物质的提取和分离效果,并对样品前处理和色谱条件进行了优化。样品中加入2-溴丙烷和1,2,4-三氯苯作内标,用乙腈超声萃取并经有机膜过滤后,用GC-MS进行测定,内标法定量。结果表明:16种有害物质在5~200 mg/L范围内线性关系良好,相关系数均不低于0.999;样品的加标回收率为80%~105%,相对标准偏差小于5.0%,检出限为0.08~1.41 mg/L。A GC-MS method was developed for the determination of 16 kinds of harmful substances(e.g.methanol,volatile halohydrocarbons,benzene homologues,the free toluene diisocyanate and hexane diisocyanate)in solvent based coatings.The extraction and separation efficiencies of targeted compounds by using organic solutions of ethyl acetate,n-hexane,tetrahydrofuran and acetonitrile were investigated.The procedure of sample pre-treatment and the conditions of instruments were optimized.The quantitative analysis of compounds were carried out by using 2-bromopropane and 1,2,4-trichlorobenzene as the internal standard,and acetonitrile as extraction reagent.The result indicated that the calibration curves of the 16 harmful substances were linear in the range of 5-200 mg/L with correlation coefficients no less than 0.999.The spiked recoveries ranged from 80% to 105% with relative standard deviations less than 5.0%.The detection limits ranged from 0.08 mg/L to 1.41 mg/L.The method was rapid,sensitive and accurate.
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