微波消解技术应用于难分解贵金属化合物的分析  

Application of microwave digestion technique to analysis of indissoluble precious metal compounds

作　　者：朱利亚[1] 赵忆宁 赵辉[1] 杨光宇[3] 黄章杰[3] 陈云江[1] 朱武勋[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]云南大学化学系,云南昆明650091

出　　处：《冶金分析》2007年第12期11-16,共6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行业标准制订基金(200608072-73);云南昆明贵金属研究所创新基金(2002-BY-01);云南昆明贵金属研究所研究与发展基金(06-RD03)

摘　　要：提出了微波密闭快速消解难分解的KAu(CN)2,KAu(CN)4,Pt(NH3)2(NO2)2,K2[Pt(NO2)4],Pt(NH3)2Cl2,Pt(NH3)4Cl2,(NH4)2PtCl6,K2PtCl4,Pt(C5H7O2)2等化合物的方法。比较了微波密闭消解法与传统分解法的条件;采用精密电化学滴定法分析了Au和Pt的含量,并与传统分析方法BS5658法(H2SO4发烟重量法)、火试金法和湿法重量法进行了结果对照。结果表明:以HCl-H2O2,HCl-HNO3分别为Au和Pt类化合物的消解试剂,于优化的消解条件下,Au和Pt的溶出率达100%;Au,Pt化合物对应消解时间分别为传统法的1/192～1/40和1/72～1/8,总分析流程均大大缩短;测得Au和Pt的含量与传统方法相吻合,相对标准偏差分别为0.01%～0.02%和0.05%～0.07%。A novel microwave closed digestion method for the decomposition of refractory compounds ofKAu（CN）2,KAu（CN）4,Pt（NH3）2（NO2）2,K2[Pt（NO2）4],Pt（NH3）2C12,Pt（NH3）4Cl2,（NH4）2PtCl6,K2PtCl4,Pt（C5H7O2）2 was developed . The dissolved conditions of the proposed method were compared with those of traditional methods. The contents of gold and platinum were determined using precise electrochemistry titration, and the analytical results were also compared with traditional analysis method BS5658（Gravimetry with H2 SO4 smoking）, fire assaying method and wet gravimetry. Results showed that the dissolution rates of gold and platinum achieved 100% with HC1 --H2 02, HC1--HNO3 as digestion reagents of gold and platiunm compounds under the optimized di- gestion conditions, respectively. Digestion time of the compounds as above was 1/192--1/40 and 1/72 --1/8 of the traditional methods, respectively. The total analytical processes were greatly shortened and the determination results of gold and platiunm were consistent with those of traditional methods, giving relative standard deviation of 0.01%--0.02% and 0.05%--0.07%.

关 键 词：微波消解 难分解贵金属化合物 分析 金 铂 

分 类 号：O655[理学—分析化学]