多元光谱拟合ICP-AES法同时测定钯中22个杂质元素

试样用HCl-HNO3溶解,采用多元光谱拟合(MSF)ICP-AES法同时测定钯中Pt、Rh、Ir等22个杂质元素,对基体钯的影响、MSF功能、元素分析谱线、背景校正、仪器分析参数等进行了研究,确定了最佳实验条件。杂质元素测定范围:Ag、Mg、Cu、Cr、Ti、Mn和Co为0.0004%～0.05%;Rh、Ru、Pb、Fe、Pt、Al、Zn、Si、Bi、Ca、Sb、Sn、Au和Ni为0.0005%～0.05%;Ir为0.001%～0.05%;方法的相对标准偏差(RSD)和加标回收率分别为1.9%～8.3%和85.3%～116.7%。此方法的测定元素包含国家标准GB/T 1420-2004钯中要求测定的全部杂质元素,满足SM-Pd 99.99合格性的判定要求,同时涵盖ASTM B589-94(2005)Grade 99.95的要求。

MSF for Determination of 22 Impurities in Palladium by ICP-AES

A new method of multi-component spectral fitting(MSF) for determination of 22 impurities in palladium by ICP-AES was developed.These impurities include Pt,Rh,Ir and so on.The samples were dissolved in HCl-HNO3 prior to the measurements.The influencing factors,such as the interference of palladium,MSF function,spectra of analyzed element,background correction and instrument parameters,were investigated.The measurement range from 0.0004% to 0.05% for Ag,Mg,Cu,Cr,Ti,Mn and Co,from 0.0005% to 0.05% for Rh,Ru,Pb,Fe,Pt,Al,Zn,Si,Bi,Ca,Sb,Sn,Au and Ni,and from 0.001% to 0.05 % for Ir.The RSD of the method was found to be 1.9%~8.3% with 85.3%~116.7% of the recovery of standard addition.Elements determined include all the impurities of palladium required by GB/T 1420-2004,can be used in SM-Pd 99.99 qualification,and can also be applied in ASTM B589-94(2005) Grade 99.95.