铅试金富集条件对KSCN滴定铜阳极泥中银的影响  

Effect of Enrichment Conditions of Lead Assay on Titrating Silver in Copper Anode Slime Titrated with Potassium Thiocyanate

作　　者：储悦 CHU Yue(School of Metallurgical Engineering,Anhui University of Technology,Ma’anshan,Anhui 243032,China)

机构地区：[1]安徽工业大学冶金工程学院,安徽马鞍山243032

出　　处：《中国无机分析化学》2022年第3期123-128,共6页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家重点实验室开放基金资助项目(GZSYS-KF-2020-008)。

摘　　要：针对铅试金重量法测定铜阳极泥中银时存在Pb、Bi、Pd、Cu和Te等元素干扰问题,建立了铅试金富集-硫氰酸钾滴定检测铜阳极泥中银的方法。选取银含量较高的代表性铜阳极泥样品,在熔渣硅酸度K=1.5,温度由900℃升至1100℃用时40 min条件下熔炼30 min,铅扣在920℃以1.0 g/min铅的速度进行灰吹,所得合粒用硝酸溶解后采用KSCN标准溶液直接滴定,优化条件下相对标准偏差(RSD)为0.42%(n=4),加标回收率在98.8%~99.5%,方法可有效避免Pb、Bi、Pd、Cu和Te等元素对银测定的影响。A novel analysis method was established for the determination of silver in copper anode slime by lead fire assay enrichment union potassium thiocyanate titration,because of lead fire assay determinating silver affected by lead(Pb),bismuth(Bi),palladium(Pd),copper(Cu),and tellurium(Te)and others.Owing to high silver content and typical example,copper anode slime was used as experimental sample.The effects of silicic-acidity,lead button quality,melting temperature,heating time,cupelling temperature and holding time on the silver content test results were studied.Results indicated that when silicic-acidity(K)was 1.5,melting time 30 min,heating time 40 min from 900℃to 1100℃,lead button cupelledat the speed of 1.0 g/min at 920℃,and the composite granule dissolved with aqua regia for the determination of silver by potassium thiocyanate titration,the relative standard deviations(RSD,n=4)of determination results were 0.42%,the recoveries were between 98.8%and 99.5%,RSD was 0.28%.This new method can effectively avoid negative impacts of elements such as Pb,Bi,Pd,Cu and Te on the determination results of silver,contributing to improving the accuracy of determining silver grade in copper anode slime.

关 键 词：铅试金 硫氰酸钾滴定 铜阳极泥 固体废弃物 银 

分 类 号：O655[理学—分析化学]