引用本文:许家慧,普学伟,施艳峰,觉玉峰.吹扫捕集-气相色谱/质谱法测定水中的乙醛、丙烯醛、丙烯腈和吡啶[J].环境监控与预警,2015,9(5):20-24
XU Jia hui,PU Xue wei,SHI Yan feng,JUE Yu feng.Simultaneous Determination of Acetaldehyde,Acrolein,Acrylonitrile and Pyridine in Water by Purge and trap Gas Chromatography Mass Spectrometry[J].Environmental Monitoring and Forewarning,2015,9(5):20-24
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吹扫捕集-气相色谱/质谱法测定水中的乙醛、丙烯醛、丙烯腈和吡啶
许家慧,普学伟,施艳峰,觉玉峰
玉溪市环境监测站,云南 玉溪 653100
摘要:
水中的乙醛、丙烯醛、丙烯腈和吡啶经吹扫捕集、解吸后,用HP-VOC毛细管色谱柱进行GC分离,用GC-MS法选择离子模式(SIM)下进行检测,外标法定量。结果表明,选择取样量25 mL,吹扫流量为40 mL/min,吹扫温度为40 ℃,吹扫时间为15 min,解吸时间为2 min,解吸温度为200 ℃,烘焙时间20 min,乙醛和吡啶质量浓度在0.025~0.60 mg/L之间,丙烯醛和丙烯腈质量浓度在0.002 5~0.10 mg/L之间时,校准曲线呈线性关系,相关系数r>0.995,乙醛、丙烯醛、丙烯腈和吡啶的方法检出限分别为0.001 6,0.001 3,0.000 5和0.002 1 mg/L。对3个不同浓度样品进行空白加标实验,测量的回收率为87.8%~114.3%,相对标准偏差(n=6)为2.51%~10.4%。对3批实际水样进行分析,其中一个废水水样加标回收率为79.2%~103.8%,相对标准偏差(n=6)为3.04%~6.39%。
关键词:  吹扫捕集  气相色谱/质谱法  乙醛  丙烯醛  丙烯腈  吡啶
DOI:
分类号:O657.7+1; O657.6; X832
文献标识码:B
基金项目:
Simultaneous Determination of Acetaldehyde,Acrolein,Acrylonitrile and Pyridine in Water by Purge and trap Gas Chromatography Mass Spectrometry
XU Jiahui,PU Xuewei,SHI Yanfeng,JUE Yufeng
Yuxi Environmental Monitoring Station,Yuxi,Yunnan 653100,China
Abstract:
A method for simultaneous determination of acetaldehyde,acrolein,acrylonitrile and pyridine in water by purge and trap gas chromatography mass spectrometry (GC MS) was reported.These compounds were concentrated by purging and trapping followed by desorption before GC MS measurement using the HP VOC capillary column for separation and selective ion mode (SIM) for MS detection.External calibration was used for quantification.The following experimental conditions were used:the sampling volume was 25 mL,purging gas flow was 40 mL/min,purging temperature was 40 ℃,purging time was 15 min,desorption time was 2min,desorption temperature was 200 ℃,and baking time was 20 min.Under this condition,it was determined that the concentrations of acetaldehyde and pyridine were between 0.025 and 0.60 mg/L,and acrolein and acrylonitrile were between 0.002 5 and 0.10 mg/L.The calibration curve showed good linearity with the correlation coefficientr>0.995.The method detection limits of acetaldehyde,acrolein,acrylonitrile and pyridine were 0.001 6,0.001 3,0.000 5 and 0.002 1 mg/L,respectively.The recovery rates ranged between 87.8% and 114.3 % in three different spiked levels.The relative standard deviation (n=6) was from 2.51% to 10.4%.Three batches of water samples were analyzed.The recovery rates ranged between 79.2% and 103.8 % for the waste water,and relative standard deviation (n=6) was from 3.04% to 6.39%.
Key words:  Purge and trap  Gas chromatography mass spectrometry  Acetaldehyde  Acrolein  Acrylonitrile  Pyridine