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中国无机分析化学:2024,14(11):1589-1594
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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
刘 伟1, 崇 彪1, 罗 仙1, 张天琦2, 刘 文2, 林 波2, 罗 雄2
(1.贵研资源易门有限公司 贵研铂业股份有限公司;2.贵研资源(易门)有限公司云南)
Determination of Iridium Content in Iridium Complex Materials by Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) with Oxidize-Coprecipitation Separation
LIU Wei1, CHONG Biao1, LUO Xian1, ZHANG Tianqi2, LIU Wen2, LIN Bo2, LUO Xiong2
(1.Sino-Platinum Metals Resources Yimen Co. Ltd.,Sino-Platinu Metals Co. Ltd.;2.Sino-Platinum Metals Resources (Yimen) Co., Ltd)
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本文已被:浏览 139次   下载 80
投稿时间:2023-07-15    修订日期:2023-07-21
中文摘要: 建立了过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,电感耦合等离子体原子发射光谱法(ICP-AES)测定铱复杂物料中铱量的方法。对样品分解的温度、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、方法精密度和方法准确度进行了研究。0.10 g~0.50 g样品与5 g的过氧化钠混匀,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,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%~101.2%,相对标准偏差(RSD,n=9)为: 0.4%~1.4%。与国标方法比对,分析结果相对偏差<1%。
中文关键词: 分析化学  氧化  共沉淀  ICP-AES  复杂物料  
Abstract:A method for determination of iridium in iridium complex materials by ICP-AES with sodium peroxide alkali fusion decomposition sample, oxidation of sodium chlorate solution , separation of iridium by tellurium -tin(II) chloride coprecipitation was established.The sample decomposition temperature, sodium chlorate oxidation and separation of iridium by tellurium coprecipitation, interference and elimination of coexisting elements, sample spiking recovery rate,the accuracy and precision of method were systemic investigated. Mixing about 0.10 g~0.50 g sample with 5 g sodium peroxide,melting in muffle furnace at 750℃ for 30 min, leaching with water after cooling,acidifying with 30% hydrochloric acid, adding sodium chlorate solution to oxidize low valent 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 has no interference with 224.268 nm iridium spectral lines.Copper interference with 224.268 nm iridium spectral line so 237.277 nm iridium spectral line should be selected to copper containing sample.The method applied to detect samples with 0.5% to 50% iridium content,the recovery rate of sample spiked is 98.4%~ 101.2%,the relative standard deviation(RSD, n=9)is 0.4%~1.4% . Compared with the national standard method, the relative deviation of the analysis results is less 1%.
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基金项目:云南省重大专项科技计划(202102AB080007);固废资源化专项(国家重点研发计划2019YFC1907505)
引用文本:
刘 伟,崇 彪,罗 仙,张天琦,刘 文,林 波,罗 雄.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[J].中国无机分析化学,2024,14(11):1589-1594.
LIU Wei,CHONG Biao,LUO Xian,ZHANG Tianqi,LIU Wen,LIN Bo,LUO Xiong.Determination of Iridium Content in Iridium Complex Materials by Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) with Oxidize-Coprecipitation Separation[J].Chinese Journal of Inorganic Analytical Chemistry,2024,14(11):1589-1594.

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