Determination of High Content Silver in Lead Powder by Flame Atomic Absorption Spectrometry under Hydrochloric Acid Medium
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摘要: 对于铅精粉中银含量高的样品，特别是银含量大于1000 μg/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3000 μg/g。Abstract: 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.
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表 1 样品前处理方法对银测定结果的影响
Table 1. The influence of the sample processing on the analytical results of Ag
方法编号 溶样使用的酸 GBW07167 GBW07172 Pb-3 银含量测定值 (μg/g) 银含量标准值 (μg/g) 银含量测定值 (μg/g) 银含量标准值 (μg/g) 银含量测定值 (μg/g) 银含量标准值 (μg/g) 方法1 双氧水+硝酸 637 626±16 893 1134±93 1172 3000±150 方法2 硝酸+氢氟酸 637 626±16 1151 1134±93 2626 3000±150 方法3 硝酸+氢氟酸+高氯酸 639 626±16 1251 1134±93 2964 3000±150 方法4 盐酸+硝酸+氢氟酸+高氯酸 636 626±16 1148 1134±93 2933 3000±150 方法5 盐酸+硝酸 591 626±16 967 1134±93 2649 3000±150 
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表 2 方法准确度和精密度
Table 2. Accuracy and precision tests of the method
测定结果 GBW07167 GBW07172 Pb-3 标准值(μg/g) 626±16 1134±93 3000±150 测量值(μg/g) 620 609 654 1181 1163 1075 2945 2916 2993 637 642 639 1130 1161 1152 2960 2920 2961 621 618 633 1124 1165 1126 3003 2926 2909 641 629 635 1108 1207 1109 2913 2952 2930 平均值(μg/g) 632 1142 2944 RSD(%) 2.0 3.2 1.0 相对误差(%) 1.0 0.7 -1.9
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