盐酸介质下火焰原子吸收光谱法测定铅精粉中的高含量银  

Determination of High Content Silver in Lead Powder by Flame Atomic Absorption Spectrometry under Hydrochloric Acid Medium

作　　者：刘高令 姜贞贞 吴文清 王祝 邵蓓 邬国栋 李明礼 

机构地区：[1]西藏自治区地质矿产勘查开发局中心实验室,西藏拉萨850033 [2]西藏自治区地质矿产勘查开发局第五地质大队,青海格尔木816000

出　　处：《岩矿测试》2016年第6期621-625,共5页Rock and Mineral Analysis

基　　金：西藏自治区科学技术厅青年科技基金

摘　　要：对于铅精粉中银含量高的样品,特别是银含量大于1000μg/g和含有机质及含硫量高的铅精粉样品,在湿法处理样品过程中因存在难溶解、易包裹、易沉淀,使得银含量的测定结果偏低。针对上述问题,本文从优化样品消解方法出发,研究了铅精矿中银的最佳分析条件。即首先用盐酸除硫,再用硝酸-氢氟酸-高氯酸溶解试样,在20%盐酸介质中,用火焰原子吸收光谱仪于波长328.07 nm测定银的含量。在此实验条件下溶矿完全,提取液清澈,无沉淀。用铅精粉国家标准物质GBW07167、GBW07172和标准样品Pb-3进行验证,方法精密度（RSD,n=12）为1.0%-3.2%,银的测定结果与其标准值吻合较好。本方法制备的样品溶液稳定性较好,分析快速,可测定的银含量高达3000μg/g。Some lead powder has a high content of silver（ 〉1000 μg / g）,organic matter and sulfur,which will result in lower Ag content during wet pretreatment because Ag is insoluble,easy to wrap,and easy to precipitate.In view of these problems,the digestion method was optimized and the optimum conditions for analyzing silver in lead concentrate were determined and are reported in this paper. Sulphur was removed by hydrochloric acid. The sample was then dissolved in nitric acid-hydrofluoric acid-perchloric acid. In 20% hydrochloric acid medium,silver content was determined by the Flame Atomic Absorption Spectrometer at the wavelength of 328. 07 nm.Under these conditions,the samples are completely digested,the extract liquid is clear and no precipitation remains. The method was tested by the lead powder national standards（ GBW07167 and GBW07172） and standard sample Pb- 3. The method has a precision of 1. 0%- 3. 2%（ RSD,n = 12）. The relative error between these results and certified values is less than 1%. The stability of the sample solution prepared by this method was good,the analysis was rapid and the silver content up to 3000 μg / g can also be measured.

关 键 词：铅精粉 银 酸溶 火焰原子吸收光谱法 

分 类 号：O657.31[理学—分析化学] O614.122[理学—化学]