高氯酸-盐酸体系-火焰原子吸收光谱法测定铅精粉中的银
Determination of Silver in Lead Concentrate Powder Samples by Flame Atomic Absorption Spectrometry in HClO4-HCl System
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摘要: 从样品分解方法入手,探讨了最佳测试条件。用盐酸-氟化氢铵-硝酸-高氯酸溶解试样,在10%的盐酸介质中,用火焰原子吸收光谱仪于波长328.1 nm处,以空气-乙炔火焰测定铅精粉中的银量,克服了用铅析或灰吹法测定的步骤冗长等缺点。用铅精粉国家一级标准物质GBW 07167分析验证,测定结果与标准值吻合。方法精密度(RSD, n=12)为2.2%~4.3%,方法检出限为1.2 μg/g。方法分析快速,简单。Abstract: In this paper, a method for the determination of silver in lead concentrate powder samples by flame atomic absorption spectrometry was developed. The sample was dissolved with HCl-(NH4)HF2-HNO3-HClO4 and in the medium of 10% HCl, Ag in the sample solution was determined by air-acetylene flame atomic absorption spectrometer at wavelength of 328.1 nm. Sample digestion condition and instrument operation parameters were also studied and optimized. The detection limit of the method was 1.2 μg/g for Ag. The reliability of the method has been tested by determination of Ag in national standard reference lead concentrate powder sample (GBW 07167) and the result is in agreement with certified value with precision of 2.2%~4.3% RSD(n=12). The method provides the advantages of high efficiency and simple operation.
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Keywords:
- HClO4-HCl /
- flame /
- atomic /
- absorption
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