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

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。

Determination of twenty-six impurity elements in pure ruthenium byinductively coupled plasma atomic emission spectrometry

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 0.9995. The detection limits of method ranged from 0.00006 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).