氢化物发生-原子荧光光谱法测定钨尾矿尾砂中的砷  

Determination of Arsenic in Tungsten Tailings by Hydride Generation-Atomic Fluorescence Spectrometry

作　　者：陈祝炳 唐碧玉 曾志平 施意华 CHEN Zhubing;TANG Biyu;ZENG Zhiping;SHI Yihua(China Nonferrous Metal(Guilin)Geology and Mineral Research Co.,Ltd.,Guilin,Guangxi 541004,China)

机构地区：[1]中国有色桂林矿产地质研究院有限公司,广西桂林541004

出　　处：《中国无机分析化学》2023年第10期1054-1058,共5页Chinese Journal of Inorganic Analytical Chemistry

基　　金：广西科学研究与技术开发计划项目(桂科AD20325011)。

摘　　要：钨尾矿尾砂中的砷会随着自然条件的变化或资源综合利用过程而发生迁移,污染存在扩大的风险,快速、准确测定钨尾矿尾砂中砷的含量,将为环境污染防治措施提供数据依据。采用盐酸、硝酸消解样品,加入硫酸消除钨对原子荧光光谱法测定砷的干扰,用抗坏血酸将砷(Ⅴ)预还原为砷(Ⅲ),在盐酸介质中,砷(Ⅲ)和硼氢化钾发生氢化反应生成砷化氢,经载气导入原子化器中测定砷量,并优化原子荧光光谱法测定条件,建立了氢化物发生原子荧光光谱法测定钨尾矿尾砂中砷的分析方法。砷的测定结果相对标准偏差(RSD,n=7)小于3%,加标回收率为93.9%~111%,同时采用钨含量与钨尾矿中钨含量相近的钨矿石成分分析标准物质做方法正确度验证,相对误差的绝对值<5%。实验结果表明,建立的方法测定钨尾矿尾砂中砷含量,具有操作简单、灵敏度高,干扰少、正确度高,测定速度快等优点。Arsenic(As) in tungsten tailings will migrate with the change of natural conditions or the comprehensive utilization of resources,and the risk of pollution expansion exists.Rapid and accurate determination of arsenic in tungsten tailings will provide data basis for environmental pollution prevention measures.In this paper,hydrochloric acid and nitric acid were used for sample digestion,sulfuric acid was added to eliminate the interference of tungsten on the determination of arsenic by atomic fluorescence spectrometry,and As(Ⅴ) was pre-reduced to As(Ⅲ) by ascorbic acid.In the medium of hydrochloric acid,As(Ⅲ) and potassium borohydride were hydrogenated to form hydrogen arsenide.Arsenic was determined by carrier gas into the atomizer,and the determination conditions of atomic fluorescence spectrometry were optimized.A method for arsenic determination in tungsten tailings by hydride generation atomic fluorescence spectrometry was established.The relative standard deviation(RSD,n=7) was less than 3%.The standard recovery was 93.9%-111%,and the accuracy was verified by the standard material of tungsten composition analysis whose content was similar to that in tungsten tailings.The absolute value of relative error was less than 5%.The experimental results showed that this method had the advantages of simple operation,high sensitivity,less interference,high accuracy and fast determination speed.

关 键 词：钨尾矿尾砂 砷 氢化物发生-原子荧光光谱法 

分 类 号：O657.31[理学—分析化学] TH744.16[理学—化学]