镍锍试金-铝共熔-电感耦合等离子体发射光谱(ICP-OES)法测定废催化剂中铑铱钌

Determination of Rhodium,Iridium and Ruthenium in Spent Catalysts by Inductively Coupled Plasma Emission Optical Spectrometry with Nickel Sulphide Fire-assay and Aluminum Eutectic

研究了废催化剂中铑、铱、钌含量的分析方法。采用镍锍试金富集,镍扣用铝共熔,然后用盐酸(1+1)分离镍和铝,沉淀用高压消解罐溶解,电感耦合等离子原子发射光谱法测定铑、铱、钌。实验结果表明,加入6 g铝镍扣在900℃的马弗炉中共熔2 h,镍扣能在盐酸(1+1)中2 h以内溶解完全,方法相对标准偏差RSD(n=7)在1.2%~7.7%,铑、铱、钌的加标回收率在96.2%~100%,方法准确、可靠,可满足交易及科研需求。

The analytical methods of rhodium,iridium and ruthenium in spent catalysts are studied.The nickel sulphide fire-assay is used for enrichment.The nickel button is melted together with aluminum,which is dissolved by hydrochloric acid solution(1+1),and the precipitate is dissolved in a high-pressure digestion tank.Inductively coupled plasma atomic emission spectrometry is used to determine rhodium,iridium and ruthenium in spent catalysts.The test results show that when 6 g aluminum and nickel buttons are co-melting in a muffle furnace at 900℃for 2 hours,the nickel buttons can be completely dissolved in hydrochloric acid(1+1)within 2 hours.The relative standard deviation RSD(n=7)of the method was between 1.2%and 7.7%.The recoveries of rhodium,iridium,and ruthenium were between 96.2%and 100%indicating that the method is accurate and reliable,and can meet the needs of trading and scientific research.