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投稿时间:2025-10-24 修订日期:2025-11-17 录用日期:2025-11-21 网络发布日期:2026-05-06
投稿时间:2025-10-24 修订日期:2025-11-17 录用日期:2025-11-21 网络发布日期:2026-05-06
中文摘要: 淤泥中氨氮的快速准确测定,对环境评价具有重要 的意义。由于目前氨氮的分析方法存在分析步骤繁琐,流程长,试剂有毒等不足,本文通过对提取条件及离心方式的优化,建立了流动注射分光光度法测定淤泥中氨氮的分析方法。在最优条件下称取20 g淤泥样品以2.0 mol/L氯化钾溶液为提取液,按照固液比为1:15,采用翻转振荡的方式提取,提取液在离心转速为4000 r/min,离心时间为15 min离心后用0.45 μm的滤膜加压过滤,采用全自动流动注射分析仪直接扣除提取剂空白测定淤泥中氨氮的含量。结果表明,氨氮的质量浓度在0~10.00 mg·L-1范围内与对应的峰面积呈线性关系,相关系数为0.9999。方法检出限为0.044 mg/kg,测定下限为0.176 mg/kg,对3个不同浓度的实际样品进行测定,测定结果的相对标准偏差为3.36%~7.17%(n=6),对两种不同淤泥样品进行加标回收,回收率为88.5%~108%,经实际样品分析,本方法与国家环境保护标准HJ634-2012氯化钾提取分光光度法测定氨氮的结果基本一致。
中文关键词: 全自动流动注射分析仪 氨氮 淤泥 氯化钾提取
Abstract:The rapid and accurate determination of ammonia nitrogen in sludge is of great significance for environmental assessment. Due to the shortcomings of cumbersome analysis steps, long processes, and toxic reagents in current ammonia nitrogen analysis methods, this article establishes a flow injection spectrophotometric method for determining ammonia nitrogen in sludge by optimizing extraction conditions and centrifugation methods. Under optimal conditions, 20 g of sludge sample was extracted using a 2.0 mol/L potassium chloride solution as the extraction solution. The solid-liquid ratio was 1:15, and the extraction was carried out by flipping and oscillating. The extraction solution was centrifuged at a speed of 4000 r/min for 15 minutes and then filtered under pressure using a 0.45 μm filter membrane. The content of ammonia nitrogen in the sludge was directly determined by subtracting the extraction agent blank using a fully automatic flow injection analyzer. The results showed that the mass concentration of ammonia nitrogen was linearly related to the corresponding peak area within the range of 0-10.00 mg·L-1, with a correlation coefficient of 0.9999. The detection limit of the method is 0.044 mg/kg, and the lower limit of determination is 0.176 mg/kg. Three different concentrations of actual samples were measured, and the relative standard deviation of the measurement results was 3.36% -7.17% (n=6). Two different sediment samples were spiked and recovered, with a recovery rate of 88.5%-108%. After actual sample analysis, this method was found to be consistent with the results of the national environmental protection standard HJ634-2012 potassium chloride extraction spectrophotometric method for the determination of ammonia nitrogen.
keywords: fully automatic flow injection analyzer Ammonia nitrogen Silt Potassium chloride extraction
文章编号: 中图分类号: 文献标志码:
基金项目:国家重点研发计划(No.2019YFC1804805);豫地科研〔2024〕2号
孙慧莹 韩瑞 张帆 李小辉 郝胜涛 申硕果 郭世豪 孟萌 邵悦馨
河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心,河南省地质科学研究所有限公司,河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心
河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心,河南省地质科学研究所有限公司,河南省地质局地质灾害防治中心,河南省地质局地质灾害防治中心
SUN Huiying HAN Rui ZHANG Fan LI Xiaohui HAO Shengtao SHEN Shuoguo GUO Shihao MENG Meng SHAO Yuexin
Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Henan Geological Science Research Institute Co,Ltd,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources
Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Henan Geological Science Research Institute Co,Ltd,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Geological Hazard Prevention and Control Center of Henan Geological Bureau,Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources
引用文本:
孙慧莹,韩瑞,张帆,李小辉,郝胜涛,申硕果,郭世豪,孟萌,邵悦馨.氯化钾提取 - 流动注射分光光度法测定淤泥中的氨氮含量[J].中国无机分析化学,2026,16(5):823-830.
SUN Huiying,HAN Rui,ZHANG Fan,LI Xiaohui,HAO Shengtao,SHEN Shuoguo,GUO Shihao,MENG Meng,SHAO Yuexin.Determination of Ammonia Nitrogen in Sludge by Flow Injection Spectrophotometry with Potassium Chloride Extraction[J].Chinese Journal of Inorganic Analytical Chemistry,2026,16(5):823-830.
孙慧莹,韩瑞,张帆,李小辉,郝胜涛,申硕果,郭世豪,孟萌,邵悦馨.氯化钾提取 - 流动注射分光光度法测定淤泥中的氨氮含量[J].中国无机分析化学,2026,16(5):823-830.
SUN Huiying,HAN Rui,ZHANG Fan,LI Xiaohui,HAO Shengtao,SHEN Shuoguo,GUO Shihao,MENG Meng,SHAO Yuexin.Determination of Ammonia Nitrogen in Sludge by Flow Injection Spectrophotometry with Potassium Chloride Extraction[J].Chinese Journal of Inorganic Analytical Chemistry,2026,16(5):823-830.

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