氧化除钌-ICP-AES法测定钌化合物中的杂质元素  

Determination of Impurity Elements in Ruthenium Compounds by Oxidation Removing Ruthenium-ICP-AES Method

作　　者：李秋莹 甘建壮 王应进 孙祺 方海燕 何姣 徐光 LI Qiu-ying;GAN Jian-zhuang;WANG Ying-jin;SUN Qi;FANG Hai-yan;HE Jiao;XU Guang(State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Sino-Platinum Metals Co.Ltd.,Sino-Platinum Metals Testing Technology(Yunnan)Co.Ltd.,Kunming 650106,China)

机构地区：[1]贵研铂业股份有限公司稀贵金属综合利用新技术国家重点实验室,贵研检测科技(云南)有限公司,昆明650106

出　　处：《贵金属》2020年第2期57-61,65,共6页Precious Metals

基　　金：工业和信息化部办公厅(工信厅科[2018]31号)行业标准研制项目(2018-0580T-YS)。

摘　　要：利用四氧化钌易挥发的特点,将钌溶液用高氯酸冒烟去除钌,用ICP-AES测定样品中杂质元素。对钌基体干扰、高氯酸用量、杂质元素分析谱线、仪器分析参数等进行了研究,确定了最佳实验条件。结果表明,采用高氯酸冒烟,可将试液中钌含量降低至50μg/mL以下,有效消除钌对杂质元素的光谱干扰。方法具有较宽的测定范围,对三氯化钌样品中20个杂质元素测定的相对标准偏差(RSD,n=9)为2.0%~3.5%,加标回收率在86.3%~118.0%之间,可满足钌化合物中杂质元素的测定要求。Taking advantage of the volatility characteristics of Ru(VIII)oxide,ruthenium is removed by fuming with perchloric acid,and the impurity elements in samples are determined by ICP-AES.The influencing factors,such as the interference of ruthenium matrix,the amount of perchloric acid,the spectra of analysis elements and instrument parameters were investigated,and the best experimental conditions were determined.The results showed that the ruthenium content in the test solution can be reduced to less than 50μg/mL by adding perchloric acid to smoke the sample,and that the spectral interference of ruthenium on impurity elements can be effectively eliminated.The method has a wide determination range.The relative standard deviations(RSD,n=9)were 2.0%~3.5%for the determination of 20 impurity elements in RuCl3 samples.The recovery rates of standard addition were 86.3%~118.0%which can meet the requirements of impurity elements determination in ruthenium compounds.

关 键 词：分析化学 钌化合物 氧化挥发 电感耦合等离子体-原子发射光谱法(ICP-AES) 杂质 

分 类 号：O657.31[理学—分析化学] O652.6[理学—化学]