Determination of Peroxide in Caprolactam and Polyether Samples by Coulometric Titration
摘 要
建立了库仑滴定法测定己内酰胺与聚醚样品中过氧化物含量的方法。铂片电极分别作电解电极对和指示电极对,以1.00 mol·L-1氯化铈溶液为支持电解质,经1.0 mA电流电解生成Ce4+后,与样品溶液中过氧化物定量发生氧化还原反应,根据法拉第电解定律,计算样品中过氧化物的含量。结果表明:标准曲线的线性范围为24.11~301.35 mg·L-1,检出限(3s)为7.2 μg·g-1。采用该方法分析实际样品,测定结果与电位滴定法的结果无显著性差异,测定值的相对标准偏差(n=5)均低于3.0%。
Abstract
Coulometric titration was established to determine the content of peroxide in caprolactam and polyether samples. Platinum electrode was served as working electrode pairs and indicating electrode pairs respectively, and 1.00 mol·L-1 of ceriumchloride solution as supporting electrolyte was electrolyzed to get Ce4+ with 1.0 mA of current. Then the redox reaction occurred quantitatively with peroxide in the sample solution, and the content of peroxide in the sample was calculated according to Faraday's law of electrolysis. The results showed that the linearity range of standard curve was 24.11-301.35 mg·L-1, with detection limit (3s) of 7.2 μg·g-1. Actual samples were analyzed, and there was no significant difference between this method and potentiometric titration. RSDs (n=5) of the determined values were less than 3.0%.
中图分类号 O657.12 DOI 10.11973/lhjy-hx202106005
所属栏目 工作简报
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收稿日期 2020/4/26
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备注卜芃,讲师,硕士,主要研究方向为化工检测,53503292@qq.com
引用该论文: BU Peng,LI Hongliang. Determination of Peroxide in Caprolactam and Polyether Samples by Coulometric Titration[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(6): 507~510
卜芃,李宏亮. 库仑滴定法测定己内酰胺与聚醚样品中过氧化物的含量[J]. 理化检验-化学分册, 2021, 57(6): 507~510
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参考文献
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【2】申圣强.聚醚中过氧化物含量测定方法的研究[J].精细石油化工进展, 2019,20(3):51-53.
【3】高希.电位滴定法测定己内酰胺中的过氧化物含量[J].合成纤维工业, 2019,42(5):85-87.
【4】周雪,吕琳.滴定法测定玉米油中过氧化值的测量不确定度评定[J].现代食品, 2019(15):163-165.
【5】刘芳,王超,杨菊,等.油脂酸价和过氧化值检测方法的研究进展[J].食品安全质量检测学报, 2019,10(14):4478-4482.
【6】WANG C, YUAN F, JIN L, et al. Evaluation of the deacetylation degree of chitosan with two-abrupt-change coulometric titration[J]. Electroanalysis, 2016,28(2):401-406.
【7】李小梅,付亚康,梁大伟.非水库仑滴定法测定锂电池电解液中游离酸的含量[J].理化检验-化学分册, 2020,56(1):97-99.
【8】谷雪贤.库仑滴定法测定羧甲基壳聚糖的含量[J].理化检验-化学分册, 2019,55(9):1073-1075.
【9】薛婷.库仑滴定法间接测定补锌片中锌[J].理化检验-化学分册, 2019,55(8):941-944.
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