碱熔-原子荧光光谱法测定钨尾矿尾砂中的锡  

Determination of Tin in Tungsten Tailings by Atomic Fluorescence Spectrometry with Alkali Fusion

作　　者：陈祝炳 唐碧玉 王蒋亮 乔小芳 黄理善 CHEN Zhubing;TANG Biyu;WANG Jiangliang;QIAO Xiaofang;HUANG Lishan(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》2024年第10期1437-1442,共6页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家重点研发计划项目(2023YFF0718005);广西科学研究与技术开发计划项目(桂科AD20325011)。

摘　　要：由于钨尾矿尾砂成分复杂,尾矿中锡含量低,传统的滴定分析方法和分光光度分析法易受钨、铜等元素的干扰,导致钨尾矿尾砂中锡的测定结果不理想。采用过氧化钠熔融钨尾矿尾砂样品,水浸取,氢氧化物沉淀分离大部分干扰元素,取上清液酸化后,选用原子荧光光谱法测定其中的锡,解决了灵敏度不足的问题,同时消除了共存钨、铜等元素对锡测定的影响,建立了原子荧光光谱法准确测定钨尾矿尾砂中锡的方法。同时考察样品处理方法、测定溶液酸度、硫脲-抗坏血酸混合还原剂和硼氢化钾浓度对原子荧光光谱法测定锡的影响,并优化原子荧光光谱法测定参数。锡的测定结果相对标准偏差(RSD,n=7)小于5%;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%,并做样品加标回收实验,加标回收率为94.5%~108%。实验结果表明,方法具有操作简单、灵敏度高,干扰少、正确度高、成本低的优点。Because of the complex composition of tungsten tailings and low tin content in the tailings,the traditional titration analysis method and colorimetric analysis method are easily interfered by tungsten,copper and other elements,resulting in unsatisfactory results.In this paper,sodium peroxide was used to melt tungsten tailings samples,water leaching,hydroxide precipitation separation of most of the interference elements,supernatant liquid acidification,atomic fluorescence spectrometrywas used for determination,which solved the problem of insufficient sensitivity,eliminated the influence of coexisting tungsten,copper and other elements on the determination of tin,and established the accurate determination of tin in tungsten tailings by atomic fluorescence spectrometry.At the same time,the influences of sample treatment method,determination of solution acidity,thiourea-ascorbic acid mixed reducing agent and potassium borohydride concentration on the determination of tin by atomic fluorescence spectrometry were investigated,and the determination parameters of atomic fluorescence spectrometry were optimized.The relative standard deviation(RSD,n=7) of the determination of tin was less than 5%.The tungsten ore composition analysis standard substance with tungsten content similar to that in tungsten tailings was used for method verification.The absolute value of the relative error was less than 5%,and the recovery rate was 94.5%—108%.This method for determining tin in tungsten tailings has the advantages of simple operation,high sensitivity,less interference,high accuracy and low cost.

关 键 词：钨尾矿尾砂 锡 原子荧光光谱法 

分 类 号：O657.31[理学—分析化学]