色谱

色谱 ›› 2019, Vol. 37 ›› Issue (10): 1124-1128.DOI: 10.3724/SP.J.1123.2019.03001

• 研究论文 • 上一篇    下一篇

顶空气相色谱法快速测定污水中氨氮含量

彭容1, 刘浩1, 柴欣生1, 蒋然2   

  1. 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
  • 收稿日期:2019-03-01 出版日期:2019-10-08 发布日期:2020-12-11
  • 通讯作者: 刘浩E-mail:feliuh@scut.edu.cn.
  • 基金资助:
    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）.

Rapid determination of ammonia nitrogen in sewage by headspace gas chromatography

PENG Rong1, LIU Hao1, CHAI Xinsheng1, JIANG Ran2   

  1. 1. State Key Lab of Pulp & Paper Engineering, South China University of Technology, Guangzhou 510641, China;
    2. Pearl River Water Resources Institute, Pear River Water Resources Commission, Guangzhou 510611, China
  • Received:2019-03-01 Online:2019-10-08 Published:2020-12-11
  • Supported by:
    Guangzhou Science and Technology Plan, a Major Project of Industry-University-Research Collaborative Innovation (No. 201704020038);Guangxi Special Project for Innovation-Driven Development (No. AA18118013-9).

PDF

131

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NH4+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0.786 mg/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。

关键词: 顶空气相色谱, 氨氮, 污水, 化学反应, CO2

Abstract: 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 NH4+ in a headspace bottle to produce a strong acid with equal molarity. Thereafter, NaHCO3 was reacted with the newly generated acid to produce CO2. In the final step, the released CO2 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.

Key words: headspace gas chromatography (HS-GC), ammonia nitrogen, sewage, chemical reaction, CO2

中图分类号: