同时测定水中乙醛、丙烯醛、丙烯腈的方法研究  

Methods for Simultaneous Determination of Acetaldehyde,Acrolein and Acrylonitrile in Water

作　　者：胡晓璇 刘茜 赵震 蔡美全 丁萌萌 常淼 邹本东 HU Xiao-xuan;LIU Qian;ZHAO Zhen;CAI Mei-quan;DING Meng-meng;CHANG Miao;ZOU Ben-dong(Beijing Chaoyang Municipal Ecological and Environmental Monitoring Center,Beijing 100025,China;Beijing Municipal Ecological and Environmental Monitoring Center,Beijing 100048,China)

机构地区：[1]北京市朝阳区生态环境监测中心,北京100025 [2]北京市生态环境监测中心,北京100048

出　　处：《化学试剂》2024年第11期98-104,共7页Chemical Reagents

摘　　要：分别建立了直接进样-气相色谱法与吹扫捕集-气相色谱/质谱法同时测定水中乙醛、丙烯醛、丙烯腈的方法。比较了两种方法测定水中3种化合物的方法性能和适用性,考察了4种不同保存条件对3种化合物测定的影响。结果表明,直接进样-气相色谱法测定3种化合物的校准曲线相关系数均大于0.997,检出限为0.02~0.05 mg/L,加标回收率为96.7%~112%,相对标准偏差为1.8%~6.1%;吹扫捕集-气相色谱/质谱法测定3种化合物的校准曲线相关系数均大于0.999,检出限均为0.5μg/L,加标回收率为95.6%~107%,相对标准偏差为1.2%~3.3%。不同保存条件实验结果显示,用盐酸调节水样pH≤2时的保存条件为最优,乙醛、丙烯醛、丙烯腈保存7 d浓度变化率分别为8.1%、7.3%、7.2%。在此保存条件下,两种方法测定地表水样品加标回收率为88.7%~110%,相对标准偏差为0.41%~5.85%;地下水样品加标回收率为86.3%~110%,相对标准偏差为0.70%~5.65%。直接进样-气相色谱法对仪器配置要求低,测定所需的样品量较少,但该方法的检出限比吹扫捕集-气相色谱/质谱法高出两个数量级。吹扫捕集-气相色谱/质谱法灵敏度更高,检出限更低,定性定量准确可靠,可满足地表水及地下水中痕量乙醛、丙烯醛、丙烯腈的监测需求。In this article,we compared the employments of the direct injection method and the purge/trap-GC-MSD method of determining acetaldehyde,acrolein,and acrylonitrile in water.In the meantime,we compared the four different preservatives of acetaldehyde,acrolein,and acrylonitrile in water.The results showed that the correlation coefficients of the three compounds were both greater than 0.997 by using the direct injection method.The detection limit ranged from 0.02 to 0.05 mg/L.The recoveries and relative standard deviations were 96.7%~112%and 1.8%~6.1%,respectively.The correlation coefficients of the three compounds were both greater than 0.999 by using the purge and trap-GC-MSD method.The detection limits were both 0.5μg/L.The recoveries and relative standard deviations were 95.6%~107%and 1.2%~3.3%.The experimental results showed that the storage conditions were optimized when the pH of the water sample was adjusted to≤2 with hydrochloric acid.Using this storage condition,the 7-day concentration changes of acetaldehyde,acrolein and acrylonitrile were 8.1%,7.3%and 7.2%,respectively.The recoveries and relative standard deviations were 88.7%~110%and 0.41%~5.85%of surface water.The recoveries and relative standard deviations were 86.3%~110%and 0.70%~5.656%of groundwater.Direct injection method is simple and requires less sample.However,the detection limit of the direct injection method was two orders of magnitude higher than the purge and trap-GC-MSD method.With a low detection limit and high recovery,the purge and trap-GC-MSD method can be thus trustable for the ultra-trace analysis of acetaldehyde,acrolein,and acrylonitrile in real water samples such as surface water and groundwater.

关 键 词：乙醛 丙烯醛 丙烯腈 直接进样 吹扫捕集 气相色谱/质谱法 保存方法 

分 类 号：X132[环境科学与工程—环境科学]