铅试金-电感耦合等离子体原子发射光谱法测定铜浸出渣中铂钯

Determination of platinum and palladium in copper leaching residue by inductively coupled plasma atomic emission spectrometry with lead fire assaying

采用铅试金法将铜浸出渣中的铂和钯捕集于金银合粒中,用硝酸（1＋7）溶解金银合粒,倾出硝酸溶解液,用王水（1＋1）溶解剩余的残渣,合并两次溶解液,加入盐酸（1＋1）沉淀银,过滤,对溶液中铂和钯进行测定,建立了电感耦合等离子体原子发射光谱法（ICP-AES）测定铜浸出渣中铂和钯的分析方法。金银合粒中金和银的干扰试验表明：在沉淀过程中不断搅拌可消除氯化银沉淀对铂和钯吸附的影响,同时溶液中的金对测定不产生干扰。方法用于铜浸出渣实际样品分析,测得结果的相对标准偏差（RSD,n=11）为5.6%-9.7%,加标回收率为94%-104%。将方法应用于铜浸出渣管理样中铂和钯的测定,测定值和参考值吻合。

Platinum and palladium in copper leaching residue were captured into gold-silver composite granule by lead fire assaying method.Then,the gold-silver composite granule was dissolved with nitric acid（1＋7）.After the solution was pouring out,the residues were dissolved with aqua regia（1＋1）.Merging the solutions above,the hydrochloric acid（1＋1）was added to precipitate the silver.After filtration,the content of platinum and palladium in filtrate was determined.Thus,a method was established for determination of platinum and palladium in copper leaching residue by inductively coupled plasma atomic emission spectrometry（ICP-AES）.The interference tests of gold and silver in gold-silver composite granule indicated that the absorption of platinum and palladium by silver chloride precipitate could be eliminated through continuous stirring in precipitation process.Meanwhile,gold in solution had no interference with the determination.The proposed method was applied to the determination of copper leaching residue actual samples.The relative standard deviations of the results（RSD,n=11）were 5.6%-9.7%,and the recoveries were between 94% and 104%.The content of platinum and palladium in control samples of copper leaching residue was determined by proposed method.The results were consistent with the reference values.