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投稿时间:2024-04-02 修订日期:2024-04-28
投稿时间:2024-04-02 修订日期:2024-04-28
中文摘要: 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比色分析法易受钨、铜等元素的干扰,导致钨尾矿尾砂中锡的测定结果不理想。本文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,解决了灵敏度不足的问题,同时消除了共存钨、铜等元素的对锡测定的影响,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%,并做样品加标回收试验,加标回收率为94%~108%。实验结果表明,本方法测定钨尾矿尾砂中锡,具有操作简单、方法灵敏度高,干扰少、正确度高,成本低的优点。
Abstract: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 of tin determination in tungsten tailings. In this paper, sodium peroxide is used to melt tungsten tailings samples, water leaching, hydroxide precipitation separation of most of the interference elements, supernatant liquid acidification, atomic fluorescence spectrometry is used for determination, which solves the problem of insufficient sensitivity, and eliminates the influence of coexisting tungsten, copper and other elements on the determination of tin, and establishes the accurate determination of tin in tungsten tailings by atomic fluorescence spectrometry. At the same time, the influence 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 is investigated, and the determination parameters of atomic fluorescence spectrometry are optimized. The relative standard deviation (RSD, n=7) of the determination of tin is less than 5%. The tungsten ore composition analysis standard substance with tungsten content similar to that in tungsten tailings is used for method verification, the absolute value of the relative error is less than 5%, and the sample spiked recovery test is done, and the recovery rate is 94%~108%. The experimental results show that the method for determining tin in tungsten tailings has the advantages of simple operation, high sensitivity, less interference, high accuracy and low cost.
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基金项目:国家重点研发计划课题(2023YFF0718005);广西科学研究与技术开发计划项目(桂科 AD20325011)
作者 | 单位 | |
陈祝炳 | 中国有色桂林矿产地质研究院有限公司 | 7237740@qq.com |
唐碧玉* | 中国有色桂林矿产地质研究院有限公司 | 187354191@qq.com |
王蒋亮 | 中国有色桂林矿产地质研究院有限公司 | 1@qq.com |
乔小芳 | 中国有色桂林矿产地质研究院有限公司 | 1@qq.com |
黄理善 | 中国有色桂林矿产地质研究院有限公司 | 1@qq.com |
引用文本:
陈祝炳,唐碧玉,王蒋亮,乔小芳,黄理善.碱熔-原子荧光光谱法测定钨尾矿尾砂中的锡[J].中国无机分析化学,2024,14(10):1437-1442.
chenzhubing,tangbiyu,WANG Jiangliang,QIAO Xiaofang,HUANG Lishan.Determination of Tin in Tungsten Tailings by Atomic Fluorescence Spectrometry with Alkali Fusion[J].Chinese Journal of Inorganic Analytical Chemistry,2024,14(10):1437-1442.
陈祝炳,唐碧玉,王蒋亮,乔小芳,黄理善.碱熔-原子荧光光谱法测定钨尾矿尾砂中的锡[J].中国无机分析化学,2024,14(10):1437-1442.
chenzhubing,tangbiyu,WANG Jiangliang,QIAO Xiaofang,HUANG Lishan.Determination of Tin in Tungsten Tailings by Atomic Fluorescence Spectrometry with Alkali Fusion[J].Chinese Journal of Inorganic Analytical Chemistry,2024,14(10):1437-1442.