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多参数分析仪测定煤化工废水总氮方法OA

Total nitrogen determination in coal chemical wastewater by multi-parameter analyzer

中文摘要英文摘要

为解决传统方法测定煤化工废水总氮操作繁琐、耗时久、试剂用量大等问题,同时满足工业批量检测需求,建立多参数分析仪耦合快速消解仪的总氮联合测定方法.以碱性过硫酸钾为消解试剂,在122℃、消解30 min的条件下,在pH=7.5咪唑缓冲体系中经镉柱还原、重氮偶联显色后在波长550 nm处测定溶液吸光度.实验结果表明,总氮质量浓度在0~1.00 mg/L范围内总氮联合测定方法的标准工作曲线线性关系良好(相关系数为 0.999 8),检出限低至0.03 mg/L,优于碱性过硫酸钾消解紫外分光光度法(HJ 636-2012)的0.05 mg/L,空白平均吸光度0.007 9;镉柱还原率为93.77%~103.64%,总氮的氧化还原率为98.0%~103.5%,加标回收率为96.3%~103.9%,不同试样总氮质量浓度的相对标准偏差为0.014%~0.191%.该方法具有高自动化程度、良好的环保经济性,优化了复杂基质废水总氮快速检测技术,可高效适配煤化工废水批量检测.

To address the problems of cumbersome operation,long analysis time,and high reagent consumption associated with traditional methods for determining total nitrogen(TN)in coal chemical wastewater,and to meet the needs for industrial batch detection,a method was established by coupling a multi-parameter analyzer with a rapid digestion instrument.Alkaline potassium persulfate was used as the digestion reagent,and the digestion condition was set at 122℃for 30 min.After cadmium column reduction in a pH=7.5 imidazole buffer system,the absorbance was measured at 550 nm after diazo coupling color development.The results demonstrated that TN concentration had a good linear relationship in the range of 0-1.00 mg/L,with a correlation coefficient R2=0.999 8 and a detection limit of 0.03 mg/L(better than 0.05 mg/L of the HJ 636-2012 standard).The average blank absorbance was 0.007 9,the cadmium column reduction rate was 93.77%-103.64%,oxidation-reduction rate of TN was 98.0%-103.5%,and the spiked recovery rate of actual samples was 96.3%-103.9%.The relative standard deviations at TN mass concentration of different sample ranged from 0.014%to 0.191%.This method is highly automated,environmentally friendly,and economical,filling the technical void in rapid TN detection of complex matrix wastewater,and is well suited for efficient application in batch monitoring of coal chemical wastewater.

李刚;杨红杰;白文娟;张峰;王奇

国家能源集团榆林化工有限公司,陕西 榆林 719000国家能源集团榆林化工有限公司,陕西 榆林 719000国家能源集团榆林化工有限公司,陕西 榆林 719000国家能源集团榆林化工有限公司,陕西 榆林 719000国家能源集团榆林化工有限公司,陕西 榆林 719000

化学化工

煤化工废水总氮多参数分析仪快速消解镉柱还原

coal chemical wastewatertotal nitrogenmulti-parameter analyzerrapid digestioncadmium column reduction

《石油化工》 2026 (6)

923-929,7

10.3969/j.issn.1000-8144.2026.06.015

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