摘要
采用氢氟酸-盐酸-硝酸-高氯酸溶解样品,硫酸铅沉淀分离,在氨水-EDTA介质中溶解硫酸铅沉淀,在乙酸-乙酸钠缓冲体系下,以二甲酚橙为指示剂,乙酸铅返滴定测定铅含量,优化了沉淀陈化时间、氨水加入量、微沸时间以及乙酸-乙酸钠缓冲溶液加入量等实验条件,建立了采用EDTA返滴定法测定铅玻璃中铅的方法。实验方法用于测定铅玻璃中铅,结果的相对标准偏差(RSD,n=11)为0.32%。按照实验方法对铅玻璃样品进行加标回收试验,回收率为99.5%~102.0%。
The sample was dissolved with hydrofluoric acid-hydrochloric acid-nitric acid-perchloric acid system.Lead was separated in the form of lead sulfate precipitate,which was then dissolved in ammoniaEDTA solution medium.The content of lead was finally determined by lead acetate back titration method in HAc-NaAc buffer solution using xylenol orange as the indicator.The experimental conditions,including the ageing time of precipitate,the addition amount of ammonia,the sub-boiling time and the dosage of HAc-NaAc buffer solution,were optimized.The determination method of lead in lead glass by EDTA back titration was established.The proposed method was applied to the determination of lead in lead glass.The relative standard deviations（RSD,n=11）of determination result was 0.32%.The recovery test of lead glass sample was conducted according to the experimental method.The recoveries were between 99.5%and 102.0%.
出处
《冶金分析》
CAS
CSCD
北大核心
2017年第2期65-69,共5页
Metallurgical Analysis
基金
北京市科技创新基地培育与发展专项(Z151100001615044)
关键词
EDTA
返滴定法
铅玻璃
铅
EDTA
back titration method
lead glass
lead
