Determination of trace gold in iron powder by high resolution continuum source flame atomic absorption spectrometry with silver protection cupellation lead fire assay enrichment
YAO Mingxing1,2,3, MAO Xiangju1,2,3, GUO Xiaorui1,2,3, SUN Qiliang1,2,3, NI Wenshan*1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China; 2. China National Engineering Research Center for Utilization of Industrial Minerals, Zhengzhou 450006, China; 3. Key Laboratory for Polymetallic Ores' Evaluation and Utilization, MNR, Zhengzhou 450006, China
Abstract：Iron powder is an important raw material for Au extraction, so it is necessary to accurately determine Au in iron powder. The self-prepared and purified basic lead carbonate was used as collector to obtain lead button by melting. Through silver protection cupellation, Au was further enriched in the silver particles. The silver particles were pressed to sheet and dissolved with HNO3 by heating. Then, the silver sheet was dissolved by adding HCl and heating. Au was fully dissolved and entered the solution. The solution was determined by high resolution continuum source flame atomic absorption spectrometry (HR-CS-FAAS) by selecting the pixel of 5. Consequently, the determination of Au in iron powder sample was realized. Two kinds of sample treatment methods, i.e., aqua regia heating-polyurethane foam adsorption separation enrichment and Ag protection cupellation lead fire assay, were compared in experiments. The results showed that the samples could not be completely dissolved by heating with aqua regia, and the determination results of Au was significantly lower than that of Ag protection cupellation lead fire assay. When the sample was treated by lead fire assay, the melting state of sample was good, and the fluidity of melting slag was also good. Au could be fully enriched in lead button. The dissolution method of Ag granule was investigated. The results showed that the Ag granule could be fully dissolved via HNO3 heating followed by HCl heating in sequence. The interference test of coexistence ions indicated that the coexistence ions did not interfere with the determination. Under the selected optimal conditions, the absorbance of Au and the corresponding mass concentration were fitted with least square method of quadratic equation to obtain the calibration curve. The linearity of the calibration curve was good, and the determination coefficient was 0.999 9. The limit of detection of method was 0.005 25 μg/g, and the limit of quantification was 0.017 32 μg/g. The proposed method was applied for the determination of actual iron powder sampled with Au content of 0.56-12.6 μg/g. The relative standard deviations (RSD, n=6) were between 2.3% and 3.7%. The spiked recoveries were between 92% and 107%, which could meet the requirement of recovery rate in national geological and mineral industry standard DZ/T 0130-2006.
姚明星, 毛香菊, 郭晓瑞, 孙启亮, 倪文山. 银保护灰吹铅试金-高分辨率连续光源火焰原子吸收光谱法测定铁粉中痕量金[J]. 冶金分析, 2022, 42(8): 48-54.
YAO Mingxing, MAO Xiangju, GUO Xiaorui, SUN Qiliang, NI Wenshan. Determination of trace gold in iron powder by high resolution continuum source flame atomic absorption spectrometry with silver protection cupellation lead fire assay enrichment. , 2022, 42(8): 48-54.
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