重氮偶联法测定水中亚硝酸盐氮的改进
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摘要
重氮偶联法作为测定亚硝酸盐氮的标准方法,因具有方法灵敏、选择性强、仪器较易获得等优点,被实验室广泛采用,但也存在测定上限较低,适用样品范围较窄等缺点。通过将显色剂中磷酸改为盐酸,把重氮试剂含量提高到国标法的3倍,明显提高亚硝酸盐氮的测定上限,即由原国标法上限的0.2 mg/L提高到0.6 mg/L,灵敏度与国标法接近,且准确度和精密度良好,6组标准溶液平行测定的相对误差为1.60%,相对标准偏差为1.34%,加标回收率为96.5%~104.9%,适用于生活污水、工业废水、地表水、养殖废水等水体的测定。
Diazo-Coupling method is widely used to determine nitrite nitrogen in laboratory with the characteristics of sensitive,selective and the instrument easy to obtain. But it has lower upper limit and narrow applicable sample range. By changing the phosphoric to hydrochliric acid in the color development reagent and increasing the diazonium reagent to three times of the national standard method,the upper limit of nitrite determination can be significantly improved. Namely,the 0. 2 mg/L of the upper limit of the GB standard curve increase to 0. 6 mg/L. The sensitivity of the improved method is approximate to that of the national standard method,in addition,its accuracy and precision are good. The relative error and the relative standard deviation of the six groups of parallel determination of standard solution is 1. 6% and 1. 34%,respectively. The recovery rate is between 96. 5%-104. 9%,which is applicable for the determination of nitrite in domestic sewage,industrial wastewater,surface water and aquaculture wastewater.
Diazo-Coupling method is widely used to determine nitrite nitrogen in laboratory with the characteristics of sensitive,selective and the instrument easy to obtain. But it has lower upper limit and narrow applicable sample range. By changing the phosphoric to hydrochliric acid in the color development reagent and increasing the diazonium reagent to three times of the national standard method,the upper limit of nitrite determination can be significantly improved. Namely,the 0. 2 mg/L of the upper limit of the GB standard curve increase to 0. 6 mg/L. The sensitivity of the improved method is approximate to that of the national standard method,in addition,its accuracy and precision are good. The relative error and the relative standard deviation of the six groups of parallel determination of standard solution is 1. 6% and 1. 34%,respectively. The recovery rate is between 96. 5%-104. 9%,which is applicable for the determination of nitrite in domestic sewage,industrial wastewater,surface water and aquaculture wastewater.
引文
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[2]LI L,CHU G S.A Study on Removal Ammonia,Nitrogen and Nitrite in Close-Cycle Aquaculture System[J].Jilin Water Resources,2010.
[3]FOESEL B U,GIESEKE A,SCHWERMER C,et al.Nitrosomonas Nm143-like Ammonia Oxidizers and Nitrospira Marina-Like Nitrite Oxidizers Dominate the Nitrifier Community in a Marine Aquaculture Biofilm[J].FEMS Microbiology Ecology,2008,63(2):192-204.
[4]贺纪正,张丽梅.氨氧化微生物生态学与氮循环研究进展[J].生态学报,2009,29(1):406-415.HE Jizheng,ZHANG Limei.Advances in AmmoniaOxidizing Microorganisms and Global Nitrogen Cycle[J].Acta Ecologica Sinica,2009,29(1):406-415.
[5]范慧群,徐乐.离子色谱法测定水中亚硝酸盐氮的方法确认[J].今日科苑,2009(9):119-120.FAN Huiqun,XU Le.Determination of Nitrite Nitrogen in Water by Ion Chromatography[J].Modern Science,2009(9):119-120.
[6]国家环境保护局.水质亚硝酸盐氮的测定气相分子吸收光谱法:HJ/T 197—2005[S].北京:中国环境科学出版社,2005.
[7]国家环境保护局.水质亚硝酸盐氮的测定分光光度法:GB 7493—87[S].北京:中国标准出版社,1987.
[8]边超,蔡五田,刘金巍,等.水中亚硝酸根的现场测定及在地下水污染调查中的应用[J].环境工程,2016,34(9):130-133.BIAN Chao,CAI Wutian,LIU Jinwei,et al.In Situ Deter Mination of Nitrite in Water and Its Application in Groundwater Contamination Investigation[J].Environmental Engineering,2016,34(9):130-133.
[9]国家环境保护总局《水和废水监测分析方法》编委会.水和废水监测分析方法[M].4版.北京:中国环境科学出版社,2002.
[10]盛骤,谢式千,潘承毅.概率论与数理统计[M].北京:高等教育出版社,2008:244-248.
[11]邓勃.关于校正曲线建立和应用中一些问题的探讨[J].中国无机分析化学,2011,1(3):1-7.DENG Bo.The Discussion on Some Problems with Construction and Application of Calibration Curve[J].Chinese Journal of Inorganic Analytical Chemistry,2011,1(3):1-7.
[12]国家环境保护部.环境监测分析方法标准制修订技术导则:HJ 168—2010[S].北京:中国环境科学出版社,2010.