硫脲析出-自动光度滴定法测定钯化合物中钯
Determination of palladium in palladium compounds by thiourea release-automatic photometric titration
金娅秋 1陶赛祥 1付仕梅 1孙祺 1张航波 1汪原伊 1何姣 1杨辉1
作者信息
- 1. 云南省贵金属新材料控股集团股份有限公司 贵研检测科技(云南)有限公司,昆明 650106
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摘要
用硫脲选择性析出钯-EDTA中的钯,用自动光度滴定法滴定与钯等量的EDTA,实现钯化合物中含钯量的测定.对方法测定波长、硫脲用量、终点突跃ΔE值、共存离子影响重要条件,以及常规滴定条件进行了系统研究.结果表明,测定 19%～60%钯含量,方法相对标准偏差(RSD,n=11)为 0.11%～0.19%,加标回收率为 99.64%～100.27%,测定结果与相关标准方法吻合.采用硫脲代替丁二肟,解决了丁二肟钯絮状沉淀包裹光度电极表面影响测定,以及采用自动光度滴定法有效解决钯棕红色影响目视终点准确判定的问题,实现钯含量的自动快速测定,提高工作效率.
Abstract
After palladium in palladium-EDTA was selectively released by thiourea,EDTA equal to the amount of palladium was analyzed by using automatic photometric titration.In this way,the determination of palladium in palladium compounds was realized.The wavelength of determination,the amount of thiourea,the value of end-point jump ΔE,the influence of coexisting ions and the conventional titration conditions were studied systematically.The results showed that when the palladium content was in the range of 19%～60%,the relative standard deviation(RSD,n=11)was 0.11%～0.19%with a spiked recovery rate of 99.64%～100.27%,consistent with the related standard methods.Choosing thiourea instead of dimethylglyoxime as a releasing agent can solve the problem arising from the precipitation of dimethylglyoxime-Pd complex on the surface of the photometric electrode,and using automatic photometric titration can eliminate the error in judging the titration end point by the visual inspection.The automatic and rapid determination of palladium content can be realized by adopting the method developed in this study.
关键词
分析化学/络合滴定-自动光度滴定法/钯/硫脲析出/EDTAKey words
analytical chemistry/complexation titration-automatic photometric titration/palladium/thiourea release/EDTA引用本文复制引用
基金项目
云南省贵金属实验室科技计划(YPML-2023050237)
出版年
2024
NETL
NSTL
万方数据