气相色谱-质谱法测定胺类固化剂中23种有害芳香胺

Determination of 23 harmful aromatic amines in amine curing agents by gas chromatography-mass spectrometry

建立了一种测定胺类固化剂中残余23种有害芳香胺含量的气相色谱-质谱分析方法。称取0.4 g胺类固化剂试样,置于50 mL样品瓶中,加入20 mL乙腈,超声提取30 min,提取液经0.22μm有机过滤器过滤后进行测定,使用DB-35MS色谱柱进行分析,气相分流比为15∶1,外标法进行定量。该方法样品处理过程简单,23种芳香胺在质量浓度为5~50 mg/L范围内线性相关系数均大于0.996,检出限均不大于71.4 mg/kg,高、中、低三个水平加标回收率为86.5%~99.4%,相对标准偏差为1.6%~7.9%(n=6),能够满足检测要求。

A method for determining the content of residual 23 harmful aromatic amines in amine curing agents has been established.0.4 g amine curing agent sample was added into a 50 mL sample bottle,then 20 mL of acetonitrile was added in sequence,exacted for 30 min with ultrasonic,the solution was filtered with 0.22μm filter membrane,the determination was carried out using a DB-35MS chromatographic column for analysis.The gas phase separation ratio was 15:1,and the external standard method was used for quantification.The pre-treatment process of this method was simple.The linear correlation coefficients of 23 aromatic amines in the range from 5 mg/L to 50 mg/L were all greater than 0.996,and the detection limits were less than 71.4 mg/kg.The recovery rates for high,medium,and low levels of spiking ranged from 86.5%to 99.4%,and the relative standard deviations ranged from 1.6%to 7.9%(n=6).The method can meet the detection requirements.