A headspace gas chromatography method was developed for the simultaneous determination of acetaldehyde,acrylaldehyde and acrylonitrile in water. Acetaldehyde, acrylaldehyde and acrylonitrile in water samples were extracted by headspace technology,then seperated with HP-innowax capillary column and detected by FID. Retention time of the peaks was used for qualitative analysis,while external standard method was used for quantitative analysis. The lowest detection limits were 0.04 mg/L for acetaldehyde, 0.02 mg/L for acrylaldehyde and 0.01 mg/L for acrylonitrile. The recovery rates were 95.2％ ～ 98.7％ for acetaldehyde, 95.8％ ～ 97.9％ for acrylaldehyde and 96.7％ ～ 99.6％ for acrylonitrile. And RSD (n = 6)were lower than 5.2％. This method is simple, rapid, accurate and applicable for determination of acetaldehyde,acrylaldehyde and acrylonitrile in various water samples.%建立水中微量乙醛、丙烯醛和丙烯腈的顶空气相色谱(HS-GC)测定方法,经项空进样,用HP-INNOWAX毛细管色谱柱程序升温分离,FID检测,以保留时间定性,外标法定量.水中乙醛、丙烯醛和丙烯腈的检出质量浓度分别为0.04,0.02和0.01 mg/L.样品加标回收率乙醛为952%～98.7%,丙烯醛为95.8%～97.9%,丙烯腈为96.7%～99.6%,6次平行测定结果的相对标准差不大于5.2%.该方法简便、快速、准确、重现性好,适合各种水中乙醛、丙烯醛和丙烯腈的同时测定.
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