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重铬酸钾氧化-滴定法测定电解锰渣中有机质的方法改进

Improvement of method for the determination of organic matter in electrolytic manganese residue by titration with potassium dichromate oxidation

  • 摘要: 电解锰渣是电解锰工业产生的主要固体废弃物,其有机质含量是评估环境风险与资源化潜力的关键参数。本文针对直接应用重铬酸钾氧化-滴定法测定电解锰渣有机质时面临的挑战,通过方法改进与条件优化,建立了适用于电解锰渣样品中有机质的测定方法。重点考察了Mn(Ⅱ)的干扰行为,确定了其允许阈值,当Mn(Ⅱ) 质量分数小于5%时,对测定结果无显著影响;通过自制冷凝回流装置,有效抑制了消解过程中试剂的挥发,滴定精密度显著提高。经系统优化,确定最佳反应条件为在170~190 ℃油浴中自沸腾起反应3.5 min。按照实验方法测定5个电解锰渣样品中有机质,结果的相对标准偏差(RSD,n=11)为0.31%~4.3%,加标回收率为98.0%~100.6%。本方法填补了电解锰渣有机质专属检测标准的空白,可为电解锰渣的环境合规性判定与资源化安全利用提供可靠技术支撑。

     

    Abstract: Electrolytic manganese residue is the major solid waste generated in the electrolytic manganese industry,and its organic matter content is a critical parameter for environmental risk assessment and resource utilization potential evaluation.Aiming at the challenges encountered when potassium dichromate oxidation-titration is directly adopted for organic matter determination in electrolytic manganese residue,an improved analytical method suitable for electrolytic manganese residue samples was established through methodological modification and conditional optimization in this study.The interference behavior of Mn(Ⅱ) was emphatically investigated,and its allowable threshold was clarified.The experimental results indicated that Mn(Ⅱ) had no significant interference on the determination results when its mass fraction was lower than 5%.A self-assembled condensation reflux device was applied to effectively inhibit reagent volatilization in digestion process,thereby greatly improving the titration precision.After systematic optimization,the optimal reaction conditions were obtained as follows:reaction for 3.5 min from boiling in an oil bath at 170-190 ℃.The contents of organic matter in 5 electrolytic manganese residue samples were determined according to the experimental method.The relative standard deviations(RSD,n=11) of determination results were between 0.31% and 4.3%,and the recoveries ranged from 98.0% to 100.6%.The proposed method filled the gap in dedicated testing standards for organic matter in electrolytic manganese residue,and it provided reliable technical support for environmental compliance evaluation and safe resource utilization of electrolytic manganese residue.

     

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