顶空气相色谱质谱法测定涂料中15种挥发性有机物的研究

Study on the Determination of 15 Volatile Organic Compounds in Coatings by Headspace Gas Chromatography-mass Spectrometry

建立了涂料中15种挥发性有机物顶空气相色谱质谱测定方法。涂料样品经顶空平衡温度和时间分别为90℃和20 min,以DB-624毛细管柱60 m×0.25 mm×1.4μm分离,采用选择离子监测模式检测,外标法定量。结果表明:15种挥发物在0.2~100μg范围内线性关系良好,相关系数均大于0.999,方法检出限为0.05 mg/kg,3个添加水平平均回收率在84.3%~98.6%之间,相对标准偏差(RSD)为3.1%~5.5%。方法前处理操作简单快速、回收率和精密度良好,适用于涂料中15种挥发性有机物同时测定。

A headspace gas chromatography-mass spectrometry(GC/MS)method for the determination of 15 volatile organic compounds in coatings was established.The samples were equilibrated at 90℃for 20 min in headspace,separated by DB-624 capillary column(60 m×0.25 mm×1.4μm),detected by Selected Ion Monitoring Mode,and quantified by external standard method.The results showed that all the 15 volatiles had good linear relationships in the concentration range of 0.2~100μg with the correlation coefficients greater than 0.999,the detection limit of the method was 0.05 mg/kg,and the average recovery rate and relative standard deviation(RSD)of the three addition levels were 84.3%-98.6%and 3.1%-5.5%,respectively.The method had simple and rapid pretreatment operation,high recovery rate and good precision,which was suitable for the simultaneous determination of 15 volatile organic compounds in coatings.