自动顶空-气相色谱法测定固体废物中丙烯腈的方法研究

建立了自动顶空-气相色谱法测定固体废物中丙烯腈含量的分析方法。采用自动顶空进样,DM-FFAP色谱柱分离,FID检测器检测,进行了顶空平衡时间和平衡温度的优化,同时对线性范围、检出限、加标回收率、精密度和稳定性等进行了实验。在80℃下,平衡时间为30 min时,该方法丙烯腈的检出限1.66μg/kg,相对标准偏差<5%,加标回收率为92.7%~101.5%。结果表明:自动顶空-气相色谱法测定固废中丙烯腈方法前处理简单快捷,无有机溶剂消耗,干扰少,准确性和重现性好,能满足GB 5085.6—2007《危险废物鉴别标准—毒性物质含量鉴别》的要求。

DETERMINATION OF ACRYLONITRILE IN SOLID WASTE BY AUTOMATIC HEADSPACE GAS CHROMATOGRAPHY

A method to determine the acrylonitrile in solid waste by automatic headspace gas chromatography was established． This method adopted the automatic headspace sampling，separated by DM-FFAP chromatographic column，and detected by FID detector． The conditions such as headspace balance time and equilibrium temperature were optimized． The linear range， detection limit，addition recovery rate，sensitivity and stability were tested． Under the conditions of 80 ℃ and balance time of 30 min，the detection limit of acrylonitrile was 1. 66 μg /kg，the relative standard deviation was under 5%，and the standard addition recovery was 92. 7% ～ 101. 5%． The results showed that this method is rapid，accurate and applicable，without consumption of organic solvents，less disturbance; its simple pretreatment can meet the requirements of Identification Standards for“Hazardous Wastes-Toxic Substance Content”( GB 5085. 6—2007) ．