EDTA滴定法测定分银渣中的铅含量
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摘要
采用氟化铵-盐酸-硝酸-高氯酸溶解样品,加入氢溴酸除去样品中的砷、锑、锡等共存元素,加入硫酸将样品中的铅转化为硫酸铅沉淀,通过过滤与其它元素分离,滴定前加入巯基乙酸掩蔽铋,在乙酸-乙酸钠缓冲体系下,以二甲酚橙为指示剂,建立了采用EDTA络合滴定法测定分银渣中铅含量的方法。实验方法用于测定分银渣中的铅含量,测定结果的相对标准偏差(RSD,n=11)为0.32%～0.90%,加标回收率为100%～102%。能够满足日常测定需求。
The sample was dissolved with ammonium fluoride-hydrochloric acid-nitric acid-perchloric acid.The coexisting elements such as arsenic,antimony and tin were separated by acid-hydrobromic acid.Then,the sulphuric acid was added to promote the formation of lead sulfate precipitation,which was separated with the other elements by filtration.Before titration,mercaptoacetic acid was added into solution to eliminate the influence of bismuth.In acetic acid-sodium acetate buffer solution,the determination method of lead content in silver separating residue by EDTA titration was established by using xylenol orange as an indicator.The proposed method was used for determination of lead content in silver separating residue.The results showed that the relative standard deviations(RSD,n=11)was between 0.32% and 0.90%.The recovery rate of the determination method was between 100% and 102%.The optimized operation process is simple and can meet the production requirements.
The sample was dissolved with ammonium fluoride-hydrochloric acid-nitric acid-perchloric acid.The coexisting elements such as arsenic,antimony and tin were separated by acid-hydrobromic acid.Then,the sulphuric acid was added to promote the formation of lead sulfate precipitation,which was separated with the other elements by filtration.Before titration,mercaptoacetic acid was added into solution to eliminate the influence of bismuth.In acetic acid-sodium acetate buffer solution,the determination method of lead content in silver separating residue by EDTA titration was established by using xylenol orange as an indicator.The proposed method was used for determination of lead content in silver separating residue.The results showed that the relative standard deviations(RSD,n=11)was between 0.32% and 0.90%.The recovery rate of the determination method was between 100% and 102%.The optimized operation process is simple and can meet the production requirements.
引文
[1]诸向东,汪洋,李仕雄,等.分银渣中有价金属高效回收利用[J].矿冶工程(Mining and Metallurgical Engineering),2012,32(6):86-89.
[2]刘秋波.自动电位滴定法测定铜冶炼分银渣中的银量[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2018,8(4):47-50.
[3]北京矿冶研究总院测试研究所.有色冶金分析手册[M].北京:冶金工业出版社,2004:160-163.
[4]向德磊.EDTA滴定法测定铅冶炼原料中铅含量结果正确度的探讨[J].冶金分析(Metallurgical Analysis),2016,36(8):35-40.
[5]方文韬,史旭峰,朱克聪.铋矿石中高含量铅的测定方法[J].云南地质(Yunnan Geology),2015,34(3):480-483.
[2]刘秋波.自动电位滴定法测定铜冶炼分银渣中的银量[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2018,8(4):47-50.
[3]北京矿冶研究总院测试研究所.有色冶金分析手册[M].北京:冶金工业出版社,2004:160-163.
[4]向德磊.EDTA滴定法测定铅冶炼原料中铅含量结果正确度的探讨[J].冶金分析(Metallurgical Analysis),2016,36(8):35-40.
[5]方文韬,史旭峰,朱克聪.铋矿石中高含量铅的测定方法[J].云南地质(Yunnan Geology),2015,34(3):480-483.