多元光谱拟合ICP-AES法同时测定钯中22个杂质元素

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

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。

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 HC1 -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 pal- ladium required by GB/T 1420 - 2004, can be used in SM - Pd 99.99 qualification, and can also be ap- plied in ASTM B589 -94（2005） Grade 99.95.