微波消解-硫酸亚铁电位滴定法测定贵金属合金中金  

Determination of gold in precious metal alloys by microwave digestion and potentiometric titration with ferrous sulfate

作　　者：朱利亚[1] 赵忆宁 李楷中[1] 杨谅孚[3] 杨光宇[4] 管有祥[1] 金娅秋[1] 安中庆[1] 刘云杰[1] 

机构地区：[1]昆明贵金属研究所,云南昆明650106 [2]云南省标准化研究院,云南昆明650228 [3]昆明冶金研究院,云南昆明650031 [4]云南大学化学系,云南昆明650091

出　　处：《冶金分析》2008年第5期14-18,共5页Metallurgical Analysis

基　　金：云南省自然科学基金(05E024M);国家标准化技术委员会国家标准制(修)订基金(No.20064001-T-610)

摘　　要：提出了硫酸亚铁电位滴定金的方法，研究了贵金属合金的微波消解和预处理方法，讨论了提高滴定Au的准确度和精密度的条件，比较了本法与原《国家标准》和火试金分析方法。结果表明：用HCl-H2O2试剂通过微波加热可快速消解金、铂、钯合金样品。CuCl预分离大量的Pt、Pd、Rh、Ir和Sn等干扰元素后，在稀HCl介质中，用FeSO4电位滴定法测定质量分数3%-99.5%的Au，相对标准偏差为0.02%-0.22%，与库仑法和火试金法的分析结果吻合。方法已成功地应用于金、铂、钯等贵金属合金、金粉、首饰、自然金、溶液、冶金物料等试样中Au的测定。A novel potentiometric titration method for determination of Au using FeSO4 as titrant was proposed. The microwave digestion and pretreatment for precious metals alloys were researched. The conditions of improving accuracy and precision for titration of Au were discussed. The proposed method was compared with former national standard of China and fire assaying method, Results indicated that the gold, platinum and palladium alloys could be decomposed rapidly in HCl-H2O2 by microwave heating digestion. A great deal of interferential elements of Pt, Pd, Rh, Ir, Sn and otherwise were preseparated with CuCl. The analytical results were accuracy and precision, with relative standard deviation 0. 019%-0. 223% for determining Au from 3% to 99.5% and were in good accord with coulometry and fire assaying method. The developed method has been satisfactorily applied to analysis of Au in Au, Pt and Pd alloys, Au powder, jeweleries, natural Au, solution, metallurgy materiels, and so on .

关 键 词：微波消解 电位滴定法 金、铂、钯合金 金 

分 类 号：TG115.31[金属学及工艺—物理冶金]