摘要
准确、高效地测定矿石中银的含量有助于矿产资源开发和矿产综合评价。通过对消解方法、消解体系、消解温度及消解时间进行探讨,确立了最佳消解条件,采用电感耦合等离子体质谱法(ICP-MS)的KED模式测定溶液中银的含量,选用铑为内标进行在线校正,以氦气为碰撞气,通过优化碰撞氦气流量及射频功率等仪器参数,消除了银的质谱干扰,提高了分析结果的准确性,建立了高压密闭消解-ICP-MS分析矿石中银的方法。对方法的检出限、精密度和正确度等技术指标进行考察,结果表明,银在0~500μg/L线性关系良好,方法检出限(3S)为0.009μg/g。方法用于国家标准物质分析,测定值与认定值基本一致,相对标准偏差RSD(n=12)为1.4%~4.2%,对实际样品进行加标回收实验,回收率为95.4%~104%。方法操作简单、分析效率高、绿色环保。
Accurate and efficient determination of silver in ores plays a vital role in the development and evaluation of mineral resources.This study established an ICP-MS method for analyzing silver in ores using high-pressure sealed digestion.Experiments on different digestion methods,systems,temperatures and times were carried out to determine the optimal digestion conditions.The KED mode of ICP-MS was employed to measure the silver content in the solution,with rhodium selected as the internal standard for online calibration and helium gas used as the collision gas.By optimizing instrument parameters like helium gas flow rate and RF power,silver mass spectrometry interference can be eliminated,improving the analytical accuracy.The method's technical indicators,including detection limit,precision and trueness,were investigated.Silver shows a good linear relationship within 0-500μg/L,with a detection limit of 0.009μg/g.The method was applied to analyze certified reference materials,yielding measured values consistent with certificated values and a relative standard deviation(RSD,n=12)of 1.4%-4.2%.Spiked recovery tests on actual samples showed recoveries of 95.4%-104%.The method is simple to operate,efficient in analysis,and environmentally friendly.
作者
李小辉
孙慧莹
程祎
毋喆
陈亚杰
刘春霞
LI Xiaohui;SUN Huiying;CHENG Yi;WU Zhe;CHEN Yajie;LIU Chunxia(Geological Hazard Prevention and Control Center of Henan Geological Bureau,Zhengzhou,Henan 450012,China;Key Laboratory of Precious Metals Analysis and Exploration Technology of Ministry of Natural Resources,Zhengzhou,Henan 450012,China)
出处
《中国无机分析化学》
北大核心
2025年第10期1644-1650,共7页
Chinese Journal of Inorganic Analytical Chemistry
基金
河南省自然资源厅2023年度自然资源科研项目(2023-3)
豫地矿科研项目([2021]Z-32)。
作者简介
李小辉,女,高级工程师,主要从事地质及环境样品分析研究。E-mail:122825954@qq.com。
