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铅试金富集—电感耦合等离子体原子发射光谱法测定含硒碲物料中的钌铑锇铱

  • 邓育宁|朱赞芳|叶文文|谭秀珍|韦圣林
  • 作者单位:
  • 广东先导稀材股份有限公司国家稀散金属工程技术研究中心|广东先导稀贵金属材料有限公司|广东先导稀贵金属材料有限公司|广东先导稀材股份有限公司国家稀散金属工程技术研究中心|广东先导稀材股份有限公司国家稀散金属工程技术研究中心
  • 基金项目:

  • isnull
  • 详细信息:

  • 作者简介:
  • 邓育宁(1987—),男,工程师,从事分析检测方面的研究工作;E-mail:yuning.deng@vitalchem.com
  • 通讯作者:
  • 谭秀珍(1990—),女,工程师,从事分析检测方面的研究工作;E-mail:tanxiuzhen456@126.com
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Determination of ruthenium,rhodium,osmium,and iridium in selenium and Tellurium-containing materials by lead fire assay enrichment-ICP-OES

  • English Author:
  • Vital Materials Co.,Limited,National Engineering and Technology Research Center of Scattered Metal|Guangdong Vital Rare and Precious Metal Materials Co.,Ltd.|Guangdong Vital Rare and Precious Metal Materials Co.,Ltd.|Vital Materials Co.,Limited,National Engineering and Technology Research Center of Scattered Metal|Vital Materials Co.,Limited,National Engineering and Technology Research Center of Scattered Metal
  • Unit:
  • 摘要
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  • 参考文献

摘要:

钌、铑、锇、铱物理化学性质优异,成为高科技领域和工业生产中不可缺少的关键材料。实验采用铅试金富集—电感耦合等离子体原子发射光谱法测定含硒碲物料中的钌、铑、锇、铱元素,即浓硫酸溶解物料去除硒、碲,加入一定量的银,经铅试金富集得到银合金粒,银合金粒采用硝酸溶解分银,滤渣经过氧化钠和氯化钠高温熔融后用浓盐酸消解,采用电感耦合等离子体原子发射光谱法测定。实验对银加入量、熔样温度、灰吹温度、过氧化钠和氯化钠加入量、仪器参数进行了优化,确定了最优实验条件。本方法测定含硒碲物料中钌、铑、锇、铱的相对标准偏差为0.29 %~1.01 %,加标回收率为96.36 %~105.77 %,精密度和准确度满足分析测试需求。

关键词:

铅试金法;电感耦合等离子体原子发射光谱;含硒碲物料;钌;铑;锇;铱

Abstract:

Ruthenium,rhodium,osmium,and iridium have excellent physical and chemical properties,and thus become indispensable key materials in the hightech and industrial sectors.In this experiment,the determination of ruthenium,rhodium,osmium,and iridium elements in selenium and tellurium-containing materials was carried out using lead fire assay enrichment-ICP-OES,that is,dissolving the material in concentrated sulfuric acid to remove selenium and tellurium,adding a certain amount of silver,obtaining silver alloy grains through lead fire assay enrichment,dissolving the silver alloy grains with nitric acid for silver separation,melting the residue after filtration with sodium hydroxide and sodium chloride at high temperature,then dissolving it with concentrated hydrochloric acid,and determining it with ICP-OES.The experiment optimized the amount of silver added,melting temperature,cupellation temperature,the amount of sodium hydroxide and sodium chloride added,and instrument parameters to determine the optimal experimental conditions.The relative standard deviations for the determination of ruthenium,rhodium,osmium,and iridium in selenium and tellurium-containing materials using this method were 0.29 %-1.01 %,the spike recovery rates were 96.36 %-105.77 %,and the precision and accuracy met the requirements of analysis and testing.

Keywords:

lead fire assay;ICP-OES;selenium and tellurium-containing materials;ruthenium;rhodium;osmium;iridium