气相色谱法测定固体废物中丙烯醛、丙烯腈和乙腈的实验研究

Determination of Acrolein,Acrylonitrile and Acetonitrile in Solid Wastes by GC-Static Headspace Method

采用静态顶空-气相色谱法测定固体废物中丙烯醛、丙烯腈和乙腈的含量。着重讨论了顶空平衡温度、平衡时间等因素对三种物质测定结果的影响,并优化了试验参数。在优化的实验条件下,丙烯醛、丙烯腈、乙腈及溶剂甲醇能完全分离,校准曲线线性范围可达1.00到100 mg/kg,方法检出限分别为0.044、0.034和0.035 mg/kg,实际样品加标回收率在90%～109%之间,相对标准偏差为3.3%～8.6%。

The static headspace technique was combined with the Gas Chromatography（GC） to determinate the content of acrolein,acrylonitrile and acetonitrile in solid wastes.This paper analyzed factors which can influence the monitoring results,such as headspace equilibration temperature,equilibration time and so on.Under these optimum experimental conditions,acrolein,acrylonitrile and acetonitrile were able to be separated from the solvent methanol and each other completely,with the calibration graphs being linear in the range 1.00 to 100 mg /kg.The detection limits was 0.044,0.034 and 0.035 mg /kg,respectively.The extraction recoveries for these compounds in real solid wastes were 90.0%-109%,while the relative standard deviation values were 3.3% ～ 8.6%.