电感耦合等离子体原子发射光谱法测定纯钌中26种杂质元素
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摘要
准确测定纯钌中杂质元素含量对于钌粉产品性能和加工工艺具有重要意义。而钌基体对于大部分杂质元素都存在严重的干扰,直接测定难以得出准确结果。试验采用盐酸-氯酸钾在高温高压条件下消解纯钌样品,选用高氯酸冒烟除去样品中钌基体以消除基体干扰,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定纯钌中Pt、Pd、Rh、Ir、Au、Al、As、Be、Bi、Ca、Cd、Co、Cu、Fe、Mg、Mn、Na、Ni、Pb、Sn、V、Zn、Mo、Ti、Ga、Zr等26种杂质元素。各元素在0.10～10μg/mL范围内与其发射强度呈线性,相关系数均大于0.9995;方法中各元素的检出限为0.00006～0.012μg/mL。按照实验方法测定纯钌粉中26种杂质元素,结果的相对标准偏差(RSD,n=5)为1.1%～9.7%。加标回收率为89%～109%;采用实验方法测定钌粉样品中杂质元素,并采用辉光放电质谱法(GD-MS)直接测定进行比对,大部分元素测定结果均相吻合。
The accurate determination of impurity elements in pure ruthenium was of great significance to the properties and processing technology of ruthenium powder products.The ruthenium matrix had serious interference with the determination of most impurity elements,so accurate results were hardly directly measured.Pure ruthenium sample was digested in hydrochloric acid-potassium chlorate system under high temperature and high pressure conditions.The ruthenium matrix in sample was removed by perchloric acid fuming to eliminate the matrix effect.Total 26 impurity elements(including Pt,Pd,Rh,Ir,Au,Al,As,Be,Bi,Ca,Cd,Co,Cu,Fe,Mg,Mn,Na,Ni,Pb,Sn,V,Zn,Mo,Ti,Ga and Zr)in pure ruthenium was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The concentration of elements in range of 0.10-10μg/mL was linear to the emission intensity with correlation coefficients higher than 0.999 5.The detection limits of method ranged from 0.000 06 to 0.012μg/mL.Twenty-six impurity elements in pure ruthenium powder were determined according to the experimental method.The relative standard deviations(RSD,n=5)of determination results were in range of 1.1%-9.7%.The spiked recoveries were between 89%and 109%.The impurity elements in ruthenium powder sample were determined according to the experimental method,and the found results of most elements were consistent with those obtained by glow discharge mass spectrometry(GD-MS).
The accurate determination of impurity elements in pure ruthenium was of great significance to the properties and processing technology of ruthenium powder products.The ruthenium matrix had serious interference with the determination of most impurity elements,so accurate results were hardly directly measured.Pure ruthenium sample was digested in hydrochloric acid-potassium chlorate system under high temperature and high pressure conditions.The ruthenium matrix in sample was removed by perchloric acid fuming to eliminate the matrix effect.Total 26 impurity elements(including Pt,Pd,Rh,Ir,Au,Al,As,Be,Bi,Ca,Cd,Co,Cu,Fe,Mg,Mn,Na,Ni,Pb,Sn,V,Zn,Mo,Ti,Ga and Zr)in pure ruthenium was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The concentration of elements in range of 0.10-10μg/mL was linear to the emission intensity with correlation coefficients higher than 0.999 5.The detection limits of method ranged from 0.000 06 to 0.012μg/mL.Twenty-six impurity elements in pure ruthenium powder were determined according to the experimental method.The relative standard deviations(RSD,n=5)of determination results were in range of 1.1%-9.7%.The spiked recoveries were between 89%and 109%.The impurity elements in ruthenium powder sample were determined according to the experimental method,and the found results of most elements were consistent with those obtained by glow discharge mass spectrometry(GD-MS).
引文
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[7]肖燕飞,黄莉,李明来,等.ICP-AES法测定离子吸附型稀土矿镁盐体系稀土浸出液中稀土与非稀土杂质[J].稀有金属,2017,41(4):390-397.XIAO Yan-fei,HUANG Li,LI Ming-lai,et al.Determination of rare earth elements and non-rare earth elements in leaching solution with magnesium salt system of ionadsorption type rare earth ore by ICP-AES[J].Chinese Journal of Rare Metals,2017,41(4):390-397.
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[10]钟跃汉,王利华,孙友宝,等.ICP-AES法测定固体废物中22种金属元素的含量[J].环境化学,2016(9):1974-1976.ZHONG Yue-han,WANG Li-hua,SUN You-bao,et al.Determination of 22metal elements in solid waste by ICP-AES[J].Environmental Chemistry,2016(9):1974-1976.
[11]冯圣雅,王瑶,李艳萍,等.ICP-AES法测定FeSiB非晶合金炉渣中Al2O3、B2O3、CaO、MgO、MnO、SiO2和TiO2[J].金属功能材料,2015(1):44-47.FENG Sheng-ya,WANG Yao,LI Yan-ping,et al.Determination of Al2O3,B2O3,CaO,MgO,MnO,SiO2 and TiO2in slag of FeSiB amorphous alloy by ICP-AES[J].Metallic Functional Materials,2015(1):44-47.
[12]全国有色金属标准化技术委员会.GB/T 33909-2017纯铂化学分析方法铂、铑、铱、钌、金、银、铝、铋、铬、铜、铁、镍、铅、镁、锰、锡、锌、硅量的测定电感耦合等离子体质谱法[S].北京:中国标准出版社,2017.
[2]全国有色金属标准化技术委员会.GB/T 23275-2009钌粉化学分析方法铅、铁、镍、铝、铜、银、金、铂、铱、钯、铑、硅量的测定辉光放电质谱法[S].北京:中国标准出版社,2009.
[3]王立平,冯海涛,董亚萍,等.标准加入ICP-AES法测定铬酸钠中杂质元素[J].光谱学与光谱分析,2015,35(2):523-526.WANG Li-ping,FENG Hai-tao,DONG Ya-ping,et al.Standard addition determination of impurities in Na2CrO4by ICP-AES[J].Spectroscopy and Spectral Analysis,2015,35(2):523-526.
[4]任传婷,徐光,唐发静,等.ICP-AES法测定钯炭中铅、铜和铁量[J].贵金属,2015,36(3):67-71.REN Chuan-ting,XU Guang,TANG Fa-jing,et al.Determination of lead,copper and iron contents in palladiumcarbon by ICP-AES[J].Precious Metals,2015,36(3):67-71.
[5]赵刚,谢璐,龙军桥,等.ICP-AES/AFS联合测定金矿地质样品中32种主次痕量元素[J].黄金,2015(1):70-74.ZHAO Gang,XIE Lu,LONG Jun-qiao,et al.Combined ICP-AES/AFS method in determining 32 major and minor elements in gold geological samples[J].Gold,2015(1):70-74.
[6]刘爽,叶晓英,杨春晟.电感耦合等离子体原子发射光谱(ICP-AES)法测定高纯铝中Fe、Cu、Mg、Zn、Ti[J].中国无机分析化学,2017,7(2):42-45.LIU Shuang,YE Xiao-ying,YANG Chun-sheng.Determination of Fe,Cu,Mg,Zn and Ti in high pure aluminum by ICP-AES[J].Chinese Journal of Inorganic Analytical Chemistry,2017,7(2):42-45.
[7]肖燕飞,黄莉,李明来,等.ICP-AES法测定离子吸附型稀土矿镁盐体系稀土浸出液中稀土与非稀土杂质[J].稀有金属,2017,41(4):390-397.XIAO Yan-fei,HUANG Li,LI Ming-lai,et al.Determination of rare earth elements and non-rare earth elements in leaching solution with magnesium salt system of ionadsorption type rare earth ore by ICP-AES[J].Chinese Journal of Rare Metals,2017,41(4):390-397.
[8]马兵兵,弥海鹏,周西林,等.微波消解-ICP-AES法测定拟薄水铝石中11种微量或痕量杂质元素[J].分析试验室,2017(2):194-197.MA Bing-bing,MI Hai-peng,ZHOU Xi-lin,et al.Determination of 11micro or trace elements in pseudoboehmite by ICPAES with microwave digestion[J].Chinese Journal of Analysis Laboratory,2017(2):194-197.
[9]曹磊,陈微微,高孝礼,等.基体干扰对ICP-AES分析土壤样品中主、次量元素的影响研究[J].光谱学与光谱分析,2016,36(7):2260-2265.CAO Lei,CHEN Wei-wei,GAO Xiao-li,et al.Research on the matrix interference on major and minor elements in soil samples with ICP-AES[J].Spectroscopy and Spectral Analysis,2016,36(7):2260-2265.
[10]钟跃汉,王利华,孙友宝,等.ICP-AES法测定固体废物中22种金属元素的含量[J].环境化学,2016(9):1974-1976.ZHONG Yue-han,WANG Li-hua,SUN You-bao,et al.Determination of 22metal elements in solid waste by ICP-AES[J].Environmental Chemistry,2016(9):1974-1976.
[11]冯圣雅,王瑶,李艳萍,等.ICP-AES法测定FeSiB非晶合金炉渣中Al2O3、B2O3、CaO、MgO、MnO、SiO2和TiO2[J].金属功能材料,2015(1):44-47.FENG Sheng-ya,WANG Yao,LI Yan-ping,et al.Determination of Al2O3,B2O3,CaO,MgO,MnO,SiO2 and TiO2in slag of FeSiB amorphous alloy by ICP-AES[J].Metallic Functional Materials,2015(1):44-47.
[12]全国有色金属标准化技术委员会.GB/T 33909-2017纯铂化学分析方法铂、铑、铱、钌、金、银、铝、铋、铬、铜、铁、镍、铅、镁、锰、锡、锌、硅量的测定电感耦合等离子体质谱法[S].北京:中国标准出版社,2017.
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