氧化-共沉淀分离-电感耦合等离子体原子发射光谱(ICP-AES)法测定铱复杂物料中的铱量  

Determination of Iridium Content in Iridium Complex Materials by Inductively Coupled Plasma Atomic Emission Spectroscopy(ICP-AES) with Oxidize-Coprecipitation Separation

作　　者：刘伟 崇彪 刘文 罗仙 张天琦 林波 罗雄 LIU Wei;CHONG Biao;LIU Wen;LUO Xian;ZHANG Tianqi;LIN Bo;LUO Xiong(Sino-Platinum Metals Resources(Yimen)Co.,Ltd.,Yuxi,Yunnan,651100,China)

机构地区：[1]贵研资源(易门)有限公司,云南玉溪651100

出　　处：《中国无机分析化学》2024年第11期1589-1594,共6页Chinese Journal of Inorganic Analytical Chemistry

基　　金：云南省重大专项科技计划项目(202102AB080007);国家重点研发计划固废资源化专项项目(2019YFC1907505)。

摘　　要：在铱复杂物料测定中,容易受到钯、铑、钌、铁、镍等共存元素的干扰。通过对样品分解温度、氯酸钠氧化铱及碲共沉淀分离条件、共存元素的干扰及消除、样品加标回收率、方法精确度和方法准确度进行研究,建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定铱复杂物料中铱量的方法。结果表明,0.10~0.50 g样品与5 g过氧化钠混匀,于马弗炉中750℃熔融30 min,冷却后用水浸出,30%盐酸酸化,加氯酸钠溶液将低价态铱氧化至+4价,用碲共沉淀法分离铱,ICP-AES法测定铱含量。测定液中共存的铂、钯、铑、钌对224.268 nm铱谱线无干扰,铜对224.268 nm铱谱线有干扰,故测定含铜样品选择237.277 nm铱谱线为分析线。方法应用于检测0.5%~50%铱量的样品,样品加标回收率98.4%~101%,相对标准偏差(RSD,n=9)为0.40%~1.4%。与国标方法比对,分析结果相对偏差<1%。氧化钠碱熔分解样品、氯酸钠溶液氧化、碲-氯化亚锡共沉淀分离铱,ICP-AES法测定铱复杂物料中铱量的方法快速、准确。In the determination of iridium complex materials,it is easy to be interfered by coexisting elements such as palladium,rhodium,ruthenium,iron and nickel.The sample decomposition temperature,conditions for co-precipitation and separation of iridium and tellurium by sodium chlorate oxidation,interference and elimination of coexisting elements,sample spiking recovery,the accuracy and precision of method were systemic investigated.Based on the above research,a method for the determination of iridium content in iridium complex materials by inductively coupled plasma atomic emission spectrometry(ICP-AES) was established.The results showed that,mixing about 0.10—0.50 g of sample with 5 g of sodium peroxide,melting in muffle furnace at 750 ℃ for 30 min,leaching with water after cooling,acidifying with 30% of hydrochloric acid,adding sodium chlorate solution to oxidize low valence iridium to+4,separation iridium by tellurium coprecipitation and determination of iridium content by ICP-AES.Platinum,palladium,rhodium,and ruthenium coexisting in the determination solution had no interference with 224.268 nm iridium spectral line.Copper had interference with 224.268 nm iridium spectral line,so 237.277 nm iridium spectral line should be selected to copper containing sample.This method was applied to detect samples with iridium content ranging from 0.5% to 50%.The standard addition recovery was ranged from 98.4% to 101%,and the relative standard deviation(RSD,n=9) was ranged from 0.40% to 1.4%.Compared with national standard methods,the relative deviation of analysis results was less than 1%.The ICP-AES method is a fast and accurate method for determining the iridium content in complex iridium materials,which involves the decomposition of samples by sodium oxide alkali melting,oxidation by sodium chlorate solution,and separation of iridium by tellurium stannous chloride co precipitation.

关 键 词：氧化 共沉淀 ICP-AES 复杂物料 铱 

分 类 号：O657.31[理学—分析化学]