多元光谱拟合校正-电感耦合等离子体原子发射光谱法测定铱化合物中19种杂质元素

Determination of nineteen impurity elements in iridium compounds by inductively coupled plasma atomic emission spectrometry with multi-component spectral fitting correction

铱化合物产品中杂质元素的准确测定,是判定产品级别的重要指标,以往常采用摄谱法进行测定,但Ca、Si、Mg、Fe、Na测定结果准确性差,周期较长。根据铱化合物易溶于水及酸的性质,采用盐酸溶解样品,电感耦合等离子体原子发射光谱法(ICP-AES)测定了三氯化铱、四氯化铱、氯铱酸、氯铱酸铵等铱化合物中Pt、Pd、Ru、Rh、Ag、Au、Cu、Fe、Zn、Ni、Mn、Mg、Al、Ca、Sn、Na、Si、Pb、K等19种杂质元素。基体Ir对Pt、Sn产生的光谱干扰采用多元光谱拟合(MSF)方法校正,杂质元素间没有干扰。方法的检出限(μg/mL)为0.078(Pt)、0.008 0(Pd)、0.014(Ru)、0.031(Rh)、0.002 9(Ag)、0.016(Au)、0.003 5(Cu)、0.012(Fe)、0.014(Zn)、0.009 8(Ni)、0.001 0(Mn)、0.002 2(Mg)、0.001 6(Al)、0.021(Ca)、0.057(Sn)、0.020(Na)、0.11(Si)、0.014(Pb)和0.008 3(K)。按照实验方法测定三氯化铱中Pt、Pd、Ru、Rh、Ag、Au、Cu、Fe、Zn、Ni、Mn、Mg、Al、Ca、Sn、Na、Si、Pb、K等19种元素,结果的相对标准偏差(RSD,n=9)为1.2%~7.4%;加标回收率在89%~114%之间。

The accurate determination of impurity elements in iridium compound products was an important index to judge the production grade.The conventional determination method was spectrography.However,the accuracy of determination results was low for Ca,Si,Mg,Fe and Na,and the analytical period was long.Based on the property of iridium compounds that they were easily dissolved in water and acid,the samples were dissolved with hydrochloric acid.Then,the content of nineteen impurity elements(including Pt,Pd,Ru,Rh,Ag,Au,Cu,Fe,Zn,Ni,Mn,Mg,Al,Ca,Sn,Na,Si,Pb and K)in iridium compounds such as iridium trichloride,iridium tetrachloride,chloroiridic acid and ammonium chloroiridate was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The spectral interference of matrix Ir with Pt and Sn was corrected by multi-component spectral fitting(MSF)correction.There was no interference among impurity elements.The detection limit(μg/mL)of method was as follows:0.078(Pt),0.008 0(Pd),0.014(Ru),0.031(Rh),0.002 9(Ag),0.016(Au),0.003 5(Cu),0.012(Fe),0.014(Zn),0.009 8(Ni),0.001 0(Mn),0.002 2(Mg),0.001 6(Al),0.021(Ca),0.057(Sn),0.020(Na),0.11(Si),0.014(Pb)and 0.008 3(K).Nineteen impurity elements(Pt,Pd,Ru,Rh,Ag,Au,Cu,Fe,Zn,Ni,Mn,Mg,Al,Ca,Sn,Na,Si,Pb and K)in chloroiridic acid were determined according to the proposed method.The relative standard deviations(RSD,n=9)of results were between 1.2%and 7.4%,and the spiked recoveries were between 89%and 114%.