基体分离-电感耦合等离子体原子发射光谱法测定辉钼精矿中痕量铼  

Determination of trace rhenium in molybdenite concentrate by matrix separation-inductively coupled plasma atomic emission spectrometry

作　　者：王景凤 WANG Jingfeng(Technology Development of Western Mining Group Co.,Ltd.,Xining 810006,China;The Engineering and Technology Research of Qinghai Western Mining Co.,Ltd.,Xining 810006,China;Qinghai Key Laboratory Plateau Comprehensive Utilization and Mineral Processing Engineering,Xining 810006,China;Qinghai Nonferrous Mineral Resources Engineering Technology Research Center,Xining 810006,China)

机构地区：[1]西部矿业集团科技发展有限公司,青海西宁810006 [2]青海西部矿业工程技术研究有限公司,青海西宁810006 [3]青海省高原矿物加工工程与综合利用重点实验室,青海西宁810006 [4]青海省有色矿产资源工程技术研究中心,青海西宁810006

出　　处：《冶金分析》2023年第1期62-67,共6页Metallurgical Analysis

基　　金：青海省科技计划项目(2022-ZJ-Y09)。

摘　　要：采用电感耦合等离子体原子发射光谱法(ICP-AES)测定辉钼精矿中铼时,钼因具有丰富的谱线,会对铼的测定产生严重的光谱干扰。为了消除基体钼对铼的干扰,实验使用30 mL硝酸-1 mL氟化氢铵-40 mL过氧化氢体系溶解样品,并将基体钼氧化成三氧化钼沉淀后过滤,选择铼的分析谱线为Re 197.312 nm,建立了基体分离-电感耦合等离子体原子发射光谱法测定辉钼精矿中痕量铼的方法。结果表明,校准曲线的线性相关系数r为0.99999,方法的检出限为0.0002%。实验方法用于测定辉钼精矿样品中铼,结果的相对标准偏差(RSD,n=6)为5.6%~6.0%。分别按照实验方法和YS/T 555.10—2009中规定的分光光度法测定钼精矿成分分析标准物质GBW07144和辉钼精矿样品中铼,结果相一致。During the determination of rhenium in molybdenite concentrate by inductively coupled plasma atomic emission spectrometry(ICP-AES),molybdenum has serious spectral interference due to its abundant spectral lines.In order to eliminate the interference of matrix molybdenum with the determination of rhenium,the sample was dissolved with 30 mL of nitric acid,1 mL of ammonium bifluoride and 40 mL of hydrogen peroxide in experiments.The matrix molybdenum was oxidized to molybdenum trioxide precipitate for filtration.Re 197.312 nm was selected as the analytical line for rhenium.The method for the determination of trace rhenium in molybdenite concentrate by ICP-AES after matrix separation was established.The results showed that the linear correlation coefficient(r)of calibration curve was 0.99999.The limit of detection was 0.0002%.The content of rhenium in molybdenite concentrate sample was determined according to the experimental method,and the relative standard deviations(RSD,n=6)of measurement results were between 5.6%and 6.0%.The content of rhenium in certified reference material(GBW07144)and sample of molybdenite concentrate was determined according to the experimental method and spectrophotometry in YS/T 555.10-2009.The found results of two methods were consistent.

关 键 词：基体分离 辉钼精矿 铼 电感耦合等离子体原子发射光谱法(ICP-AES) 钼 

分 类 号：O657.31[理学—分析化学] TF031[理学—化学]