NH3-邻苯二醛- na2so3反应流动注射分光光度法测定水中氨氮

Ying Liang, Chunmei Yan, Qing Guo, Jin Xu, Hongzhi Hu
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引用次数: 39

摘要

NH3-邻苯二醛(OPA) - na2so3反应产物在pH > 10.4时呈玫瑰红,其最大吸收波长为550 nm。在此基础上,建立了流动注射分光光度法测定水中氨氮的新方法。基于单变量实验设计,在整个实验过程中对流动注射方法和反应相关的实验参数进行了优化。线圈长度优化为1.6 m,用于储存标准溶液或样品溶液。着色液上料流速最佳值为8.20 mL/min。OPA浓度为1.06 g/L,亚硫酸盐浓度为0.050 g/L,反应pH为10.80。反应温度和停流时间影响该方法的性能。在反应温度为55℃、停流时间为340 s时,该方法的线性范围为0.100 ~ 0.700 mmol/L,检出限为0.007 mmol/L。样品吞吐量大于8 h−1。在最佳试验条件下,对湖水、河水、地下水和污水的回收率分别为100.4%、95.2%、101.7%和92.4%。用该方法和吲酚蓝法对两个湖泊水样进行了分析,结果表明两种方法之间无显著差异。与其他分光光度法测定氨氮的方法相比,该方法具有简便、可靠、重现性好、样品通量高的优点。
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Spectrophotometric determination of ammonia nitrogen in water by flow injection analysis based on NH3- o-phthalaldehyde -Na2SO3 reaction

The product of the NH3- o-phthalaldehyde (OPA) -Na2SO3 reaction is rose red at pH more than 10.4, and its maximum absorption wavelength is 550 nm. Based on this, a novel spectrophotometric method with flow injection analysis has been established to determine ammonia nitrogen in water. Experimental parameters related to the flow injection method and the reaction were optimized throughout the experiments based on univariate experimental design. The length of coil is optimized as 1.6 m for storing up standard or sample solution. The optimal value is 8.20 mL/min for loading flow rate of coloring solution. The OPA concentration, sulfite concentration and reaction pH are chosen as 1.06 g/L, 0.050 g/L and 10.80, respectively. The reaction temperature and stop flow time affects the performances of the method. The linearity range and detection limit of the proposed method are 0.100–0.700 mmol/L and 0.007 mmol/L at the reaction temperature of 55 °C and stop flow time of 340 s, respectively. The sample throughput is more than 8 h−1. Under the optimal experimental conditions, the recovery is 100.4%, 95.2%, 101.7% and 92.4% for the lake water, river water, groundwater and sewage, respectively. Two lake water samples were analyzed using both the proposed method and indophenol blue method, the results show no significant difference between these two methods. In comparison with other spectrophotometric determination method of ammonia nitrogen, the main merits of the proposed method are simplicity, reliability, reproducibility and high sample throughput.

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