结晶陈化技术在滴定分析铅阳极板中银含量的应用  

Application of Crystallization Aging Technology in Titration Analysis of Silver Content in Lead Anode Plate

作　　者：张明 ZHANG Ming(Zhuzhou Smelter Group Co.,Ltd.,ZhuZhou 412000,China)

机构地区：[1]株洲冶炼集团股份有限公司,湖南株洲412000

出　　处：《湖南有色金属》2023年第4期99-102,共4页Hunan Nonferrous Metals

摘　　要：试样用硝酸(1+4)溶解,逐步降温使其结晶,静置过夜使晶体充分长大,降低铅离子在溶液中的浓度,抑制其干扰,过滤后,在强酸介质中,加入三价铁离子指示剂,用硫氰酸钾标准溶液滴定铅阳极板中的Ag含量。该方法结果稳定、准确度高,试验加标回收率在99.84%~100.03%之间,相对标准偏差小于0.33%,测定范围在2000~20000 g/t之间具有合乎要求的线性和相关度,用火试金富集-重量法对照得到的结果。The sample is dissolved in nitric acid(1+4),and the supersaturation of lead nitrate solution is utilized to crystallize by cooling.The crystal is allowed to fully grow by standing overnight,reducing the concentration of lead ions in the solution and suppressing their interference.In a strong acid medium,a trivalent iron ion indicator is added,and the Ag content in the lead anode plate is titrated with potassium thiocyanate standard solution.This method is simple,accurate,and precise,with a recovery rate of 99.84%to 100.03%and a relative standard deviation of less than 0.33%,meeting the requirements of all parties.The determination range is between 2000~20000 g/t,with satisfactory linearity and accuracy.The results obtained are compared with the fire assay enrichment weight method.

关 键 词：直接滴定法 过饱和结晶 陈化 

分 类 号：TG115.3[金属学及工艺—物理冶金]