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    基于碳点变色性能的紫外-可见分光光度法测定脱硫液和废水中硫离子的含量

    Determination of Sulfur Ion in Desulfurization Solution and Waste Water by UV-Vis Spectrophotometry Based on Carbon Dots with Discoloration Property

    • 摘要: 以柠檬酸为碳源,尿素为氮源,采用水热法合成了具有变色性能的碳点(CDs),利用该CDs与S2-的褪色反应,提出了紫外-可见分光光度法(UV-Vis)测定脱硫液和废水中S2-含量的方法。通过循环预处理系统分离样品中的S2-,分取0.5 mL待测样品溶液和4.5 mL 100 mg·L-1CDs溶液,混匀,将酸度调节至pH 8,于30 ℃反应15 min,快速冷却至室温,采用U V-Vis测定反应前后体系在610 nm处的吸光度。结果表明,该CDs变色是氧化导致的。在pH 8条件下,S2-使CDs发生选择性褪色反应;S2-的质量浓度在0.05~1.00 mg·L-1和1.00~15.00 mg·L-1内与对应的吸光度差值呈线性关系,检出限(3S/N)为0.043 mg·L-1和0.073 mg·L-1;对实际样品进行加标回收试验,回收率为98.0%~106%,测定值的相对标准偏差(n=6)为0.92%~1.1%。方法用于实际脱硫液和废水样品分析,并与国家标准GB/T 16489-1996进行比对,结果显示两种方法的测定结果无显著性差异。

       

      Abstract: The carbon dots (CDs) with discoloration property was synthesized by hydrothermal method using citric acid as carbon source and urea as nitrogen source. Based on the discoloring reaction between CDs and S2-, a method for the determination of S2- in desulfurization solution and waste water by UV-Vis spectrophotometry was proposed. The cyclic pretreatment system was used to separate S2- from the sample. An aliquot (0.5 mL) of the sample solution for test and 4.5 mL of 100 mg·L-1CDs solution were mixed well, and the acidity was adjusted to pH 8 for reaction at 30 ℃ for 15 min, then the mixed solution was rapidly cooled to room temperature. The absorbance of the system at 610 nm was determined by UV-Vis spectrophotometry before and after the reaction. It was shown that the discoloration of CDs was caused by oxidation, and the selective discoloring reaction of CDs was induced by S2- at pH 8. Linear relationships between values of mass concentration of S2- and corresponding difference of absorbance were kept in the ranges of 0.05-1.00 mg·L-1 and 1.00-15.00 mg·L-1, with detection limits (3S/N) of 0.043 mg·L-1and 0.073 mg·L-1. Test for recovery was made on the actual samples, giving results of in the range of 98.0%-106%, with RSDs (n=6) of the determined values ranged from 0.92% to 1.1%. This method was applied to the analysis of the actual desulfurization solution and waste water samples, and there was no significant difference with GB/T 16489-1996.

       

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