高氯酸挥硒-电感耦合等离子体原子发射光谱法测定粗硒中铂和钯  

Determination of platinum and palladium in crude selenium by inductively coupled plasma atomic emission spectrometry after selenium volatilization with perchloric acid

作　　者：袁齐 左鸿毅 朱赞芳 YUAN Qi;ZUO Hongyi;ZHU Zanfang(Guangdong Shaoguan Quality and Metrology Supervision and Testing Institute,Shaoguan 512023,China;Shenzhen Zhongjin Lingnan Nonfemet Co.,Ltd.Shaoguan Smelter,Shaoguan 512024,China;Vital Materials Co.,Limited,Qingyuan 511500,China)

机构地区：[1]广东省韶关市质量计量监督检测所,广东韶关512023 [2]深圳中金岭南有色金属股份有限公司韶关冶炼厂,广东韶关512024 [3]广东先导稀材股份有限公司,广东清远511500

出　　处：《冶金分析》2024年第11期53-59,共7页Metallurgical Analysis

基　　金：国家重点专项(2019YFF0217103);全国有色金属标准化技术委员会行业标准制订项目(2022-0444T-YS)。

摘　　要：铂和钯是价格较高的贵金属元素,粗硒中铂和钯含量是贸易结算的重要指标,准确测定粗硒中铂和钯含量意义重大。选择王水溶解样品,采用高氯酸冒烟挥硒消除硒基体干扰,在10%王水中,以Pt265.945nm、Pd360.955nm为铂和钯的分析谱线,建立了高氯酸挥硒-电感耦合等离子体原子发射光谱法(ICP-AES)测定粗硒中铂和钯的方法。试验表明,1.0g样品需要加入15mL王水可溶解完全,加入10mL高氯酸高温挥发可将大部分硒基体除去,少量残余的硒基体和其他少量共存元素不干扰测定;全过程采用称重法以减少体积计算法带来的人为误差和量具误差。铂、钯的含量在0.02~15.0μg/g范围内与其对应的发射光谱强度呈线性关系,校准曲线的线性相关系数分别为0.99993和0.99998;铂和钯的检出限分别为0.000094%和0.00011%,定量限分别为0.00031%和0.00033%。采用实验方法对粗硒中铂、钯进行测定,结果的相对标准偏差(RSD,n=7)小于5%;测定结果与氧化焙烧-铅试金-电感耦合等离子体原子发射光谱法测定结果一致,精密度与正确度优于常规体积计算法。粗硒样品中铂、钯的回收率分别为98%~105%和99%~104%。Platinum and palladium are precious metal elements with high price.The contents of platinum and palladium in crude selenium is an important indicator for trade settlement,so it is of great significance to accurately determine the contents of platinum and palladium in crude selenium.In this study,a method for the determination of platinum and palladium in crude selenium by inductively coupled plasma atomic emission spectrometry(ICP-AES)after selenium volatilization with perchloric acid was established.The samples were dissolved in aqua regia.The interference of selenium matrix was eliminated by perchloric acid smoke to volatilize the selenium.Pt 265.945 nm and Pd 360.955 nm were used as the analytical lines for the determination in the medium of 10%aqua regia.The results showed that 1.0 g of sample could be completely dissolved by adding 15 mL of aqua regia.Most of the selenium matrix could be removed by adding 10 mL of perchloric acid for volatilization at high temperature.A small amount of residual selenium matrix and other coexisting elements had no interference with the measurement.The weighing method was adopted during whole test to reduce the personal error and measurement instrument error caused by volume calculation method.The content of platinum and palladium in range of 0.02-15.0μg/g was linear to the corresponding intensity.The correlation coefficients were 0.99993 and 0.99998,respectively.The limits of detection for platinum and palladium were 0.000094%and 0.00011%,and the limits of quantification were 0.00031%and 0.00033%,respectively.The experimental method was used to determine platinum and palladium in crude selenium,the relative standard deviations(RSD,n=7)were less than 5%.The measured results were consistent with those obtained by oxidizing roasting-lead fire assay-ICP-AES.The precision and trueness were superior to the conventional volume calculation method.The recoveries of platinum and palladium in crude selenium sample were 98%-105%and 99%-104%,respectively.

关 键 词：高氯酸 挥发 电感耦合等离子体原子发射光谱法(ICP-AES) 粗硒 铂 钯 

分 类 号：O657.31[理学—分析化学] TF843.5[理学—化学]