高温高压消解-ICP-AES法测定铱粉中15个杂质元素

在高温高压条件下用盐酸-氯酸钾消解铱粉样品，采用电感耦合等离子体-原子发射光谱法(ICP-AES)测定其中的15个杂质元素。进行了光谱干扰研究、谱线选择、加标回收、精密度以及基体匹配对比实验。结果表明，铱基体对个别杂质元素的某些谱线有光谱干扰；通过选取合适的测定波长及扣除合适的背景点可以消除大部分光谱干扰。方法的测定范围为0.001%~0.10%，加标回收率为87%~109%，相对标准偏差(精密度)为0.8%~6.9%，直接测定与基体匹配测定结果相当。方法可满足铱粉中铂、钯、铑、钌、金、银、铜、铁、镍、铝、铅、锰、镁、锡和锌等15个杂质元素的测定要求。

Determination of 15 Impurities in Iridium Powder with High Temperature and High Pressure Digestion by ICP-AES

Iridium powder samples were digested by hydrochloric acid and potassium chlorate under high temperature and high pressure. 15 impurities were determined by inductively coupled plasma atomic emission spectrometry. Spectral interference, selection of spectral lines, method recovery, precision experiments and matrix matching experiment were investigated. The results showed that the iridium matrix had serious spectral interference on some spectral lines of some impurities, and that the spectral interference was eliminated by selecting an appropriate wavelength and background points. The determination range of impurity elements is from 0.001% to 0.10%, and their recovery rates of standard addition are 87%~109%, and the relative standard deviation (precision) is 0.8% to 6.9%. The direct determination is equivalent to the matrix matching determination. The method can meet the determination requirements of platinum, palladium, rhodium, ruthenium, gold, silver, copper, iron, nickel, aluminum, lead, manganese, magnesium, tin and zinc impurities in iridium powder samples.