摘要
针对锗精矿分析过程中样品难溶解、锗易损失以及滴定法测定流程复杂等难点,建立了碱熔-电感耦合等离子体原子发射光谱(ICP-AES)法测定锗精矿中锗含量的分析方法。通过考察仪器的工作条件、不同的溶样方式、熔样温度和时间、介质酸度、共存元素对测定结果的影响,确定了最佳的实验条件,采用过氧化钠在700℃熔融15 min,用硝酸浸取进行前处理,在电感耦合等离子体原子发射光谱仪上选择209.426 nm作为分析谱线,仪器在200 nm处光谱的实际分辨率小于0.01 nm,在10%的硝酸介质中采用钠基体匹配的方式进行测定。实验结果表明,方法中仪器的短期稳定性小于1.5%,工作曲线具有良好的线性相关性,相关系数为0.99993,方法的检出限是0.023μg/mL。同时,选择了两个锗精矿国家标准样品GSB 04-3358-2016(Ge 4.91%)和GSB 04-3361-2016(Ge 23.57%)进行分析,分析结果与标准值基本一致,无显著性差异,相对标准偏差在0.42%~1.3%,加标回收率在98.1%~102%,方法具有较好的精密度和稳定性,能够满足锗精矿中锗含量1%~25%的快速准确测定。
To solve the problems that the germanium concentrate sample is difficult to dissolve,germanium is easy to be lost and the process of titration is too complex in the detection of germanium concentrate,a method for determination of germanium elements in germanium concentrates by inductively coupled plasma atomic emission spectrometry with alkali fusion was established in this study.Through investigating the working conditions of the instrument,different sample dissolution methods,sample melting temperature and time,medium acidity,and the effects of coexisting elements,the optimal experimental conditions were determined.The alkali fusion at 700℃for 15 minutes by sodiun peroxide and leaching nitric acid were used for pre-treatment;and 209.426 nm was selected as the analytical spectral line in ICP-AES,so that the actual resolution of the instrument′s spectrum at 200 nm was less than 0.01 nm,the sodium matrix matching method was used in 10%nitric acid medium for determination.Under the experimental conditions,the results showed that the short-term stability of the instrument was less than 1.5%,with good linear correlation-a correlation coefficient of 0.99993,and the detection limit was 0.023μg/mL in the method.At the same time,two national standard samples of germanium concentrate GSB 04-3358-2016(Ge 4.91%)and GSB 04-3361-2016(Ge 23.57%)were selected for analysis,and the results were basically consistent with the standard values without significant differences.Precision and recovery tests were conducted,with the relative standard deviations ranging from 0.42%to 1.3%,and the recoveries ranging from 98.1%to 102%.The method was of high accuracy and good precision,and it can be used in the rapid and accurate determination of germanium elements in germanium concentrates with a content range from 1%to 25%.
作者
方迪
苏春风
孙梦荷
FANG Di;SU Chunfeng;SUN Menghe(BGRIMM MTC Technology Co.,Ltd.,Beijing 102628,China)
出处
《中国无机分析化学》
CAS
北大核心
2023年第8期869-874,共6页
Chinese Journal of Inorganic Analytical Chemistry
基金
国家重点研发计划项目(2021YFC2903101)。
