湿法消解-火焰原子吸收光谱法测定铋精矿中银含量  

Determination of silver in bismuth concentrate by wet digestion and flame atomic absorption spectrometric method

作　　者：吴卓葵 张胜 WU Zhuokui;ZHANG Sheng(Center for Industrial Analysis and Testing,Guangdong Acadamy of Sciences,Guangzhou 510650,China)

机构地区：[1]广东省科学院工业分析检测中心,广东广州510650

出　　处：《中国有色冶金》2024年第5期54-59,共6页China Nonferrous Metallurgy

基　　金：广东省科技专项资金(“大专项+任务清单”)新型电子废弃物中贵金属短流程提取技术研究及应用示范项目(1421969001)。

摘　　要：由于铋精矿中含有大量的硫元素和硅元素,测定铋精矿中银的含量时,王水无法将其完全消解,导致样品溶解不完全,使得测量结果偏低。本研究采取在样品前处理加入高氯酸与氟化氢铵的方法来消解硫元素和硅酸盐化合物,然后采用火焰原子吸收光谱仪(AAS)测定铋精矿中银的含量,有效解决了铋精矿中较高的硫含量和硅含量对样品溶解及测定过程中的影响。试验过程中,采用2.0 mL高氯酸、0.2 g氟化氢铵、王水体系溶解铋精矿,在体积比20%HCl介质条件下,利用火焰原子吸收光谱仪测得铋精矿样品中的银含量,结果表明,本试验方法检出限为0.0066μg/mL,低于测定下限0.022μg/mL,表明本试验方法可行,能够满足铋精矿中银含量的测定要求;利用该方法测定样品中银含量,相对标准偏差(RSD,n=7)为0.20%~1.95%,加标回收率为97.7%~105.0%;综合元素干扰测定过程中没有产生明显的基体效应干扰。该方法适用于铋精矿中50.0~10000.0 g/t银的测定,为企业和检测机构开展铋精矿中银含量的测定提供了一种更为简便、实用性更强的分析检测方法。Due to the large amount of sulfur and silicon elements in bismuth concentrate,the silver content in bismuth concentrate can not be completely dissolved by aqua regis,resulting in incomplete sample dissolution,which may result in low measurement results.In this study,perchloric acid and ammonium bifluoride were added in sample pretreatment to dissolve sulfur and silicate compounds,and then the content of silver in bismuth concentrate was determined by flame atomic absorption spectrometer(AAS),which effectively solved the influence of high sulfur and silicon content in bismuth concentrate on sample dissolution and determination.During the test,bismuth concentrate was dissolved with 2.0 mL perchloric acid,0.2 g ammonium bifluoride and aqua regis system.Under the condition of 20%HCl medium,the silver content of bismuth concentrate samples was measured by flame atomic absorption spectrometer.The results showed that the detection limit of this test method was 0.0066μg/mL.It is lower than the lower limit of 0.022μg/mL,which indicates that this test method is feasible and can meet the determination requirements of silver content in bismuth concentrate.The relative standard deviation(RSD,n=7)was 0.20%to 1.95%,and the recoveries were 97.7%to 105.0%.There is no obvious matrix effect interference in the synthetic element interference determination.The method is suitable for the determination of 50.0 g/t~10000.0 g/t silver in bismuth concentrate,which provides a more simple and practical method for enterprises and testing institutions to determine the silver content in bismuth concentrate.

关 键 词：高硫高硅铋精矿 银含量测定 火焰原子吸收光谱法 氟化氢铵 高氯酸 消解完全 

分 类 号：TF03[冶金工程—冶金物理化学] TF817