顶空气相色谱法快速测定污水中氨氮含量  

Rapid determination of ammonia nitrogen in sewage by headspace gas chromatography

作　　者：彭容 刘浩[1] 柴欣生[1] 蒋然 PENG Rong;LIU Hao;CHAI Xinsheng;JIANG Ran(State Key Lab of Pulp & Paper Engineering,South China University of Technology,Guangzhou 510641,China;Pearl River Water Resources Institute,Pear River Water Resources Commission,Guangzhou 510611,China)

机构地区：[1]华南理工大学制浆造纸工程国家重点实验室,广东广州510641 [2]珠江水利委员会珠江水利科学研究所,广东广州510611

出　　处：《色谱》2019年第10期1124-1128,共5页Chinese Journal of Chromatography

基　　金：广州市科技计划产学研协同创新重大专项(201704020038);广西创新驱动发展专项(AA18118013-9)~~

摘　　要：研究了一种基于化学反应型顶空气相色谱的快速检测污水氨氮含量新方法。首先在顶空瓶中用过量的甲醛与NH+4反应产生等物质的量的强酸,再用NaHCO3与新生成的酸反应产生CO2,最后经过气相色谱定量CO2,间接得出样品中氨氮的含量。结果表明,氨氮含量与气相色谱信号值之间存在良好的线性相关性,相关系数为0.999,定量限为0.786mg/L(以N的质量浓度计),相对标准偏差小于2%,加标回收率在95%~105%之间。与国标纳氏试剂法相比,该方法测定结果的相对偏差在±5%以内。该方法检测效率高,适用于快速批量检测污水中氨氮的含量。This paper reports a novel method for the rapid determination of ammonia nitrogen in sewage by headspace gas chromatography (HS-GC) through a chemical reaction.During the experiment, formaldehyde, initially in excess, was reacted with NH + 4 in a headspace bottle to produce a strong acid with equal molarity.Thereafter, NaHCO 3 was reacted with the newly generated acid to produce CO 2.In the final step, the released CO 2 was determined using a gas chromatograph equipped with a thermal conductivity detector.Good linear correlation between the ammonia nitrogen content and the gas chromatographic signals was achieved.The observed correlation coefficient was 0.999, and the limit of quantification (LOQ) was 0.786 mg/L (measured based on the mass concentration of N).The relative standard deviation of reproducibility was less than 2%, and the standard recovery was between 95% and 105%.Compared with Nassar’s reagent method, the relative deviation of this method is within ±5%.This method has high detection efficiency and is suitable for the rapid batch detection of ammonia nitrogen in sewage.

关 键 词：顶空气相色谱 氨氮 污水 化学反应 CO2 

分 类 号：O658[理学—分析化学]