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| 银碲保护－铋试金灰吹－ICP-MS测定地质样品中的贵金属 |
| Determination of precious metals in geological samples by ICP-MS following bismuth fire assay under the protection of silver tellurium |
| Received:June 06, 2022 |
| DOI： |
| 中文关键词: 分析化学 铋试金 二次灰吹 保护剂 贵金属 电感耦合等离子体质谱法(ICP-MS) |
| 英文关键词: analytical chemistry bismuth assay secondary cupellation protection cupellation precious metals ICP-MS |
| 基金项目:豫自然资函[2021]157号-4；豫地矿勘查[2021]03 |
| Author Name | Affiliation | | LAI Xinze | Rock and Mineral Testing Center of Henan Province, Key Laboratory of Precious MetalsAnalysis and Exploration Technology of Ministry of Natural Resources, Zhengzhou 450012, China | | WANG Lin | Rock and Mineral Testing Center of Henan Province, Key Laboratory of Precious MetalsAnalysis and Exploration Technology of Ministry of Natural Resources, Zhengzhou 450012, China | | HU Jiazhen | Rock and Mineral Testing Center of Henan Province, Key Laboratory of Precious MetalsAnalysis and Exploration Technology of Ministry of Natural Resources, Zhengzhou 450012, China | | LAI Jiayi | No.2 Institute of Geological & Mineral Resources Survey of Henan, Zhengzhou 450012, China | | GUO Jiafan | Rock and Mineral Testing Center of Henan Province, Key Laboratory of Precious MetalsAnalysis and Exploration Technology of Ministry of Natural Resources, Zhengzhou 450012, China | | CHEN Haofeng | Rock and Mineral Testing Center of Henan Province, Key Laboratory of Precious MetalsAnalysis and Exploration Technology of Ministry of Natural Resources, Zhengzhou 450012, China | | GAO Zhijun | Rock and Mineral Testing Center of Henan Province, Key Laboratory of Precious MetalsAnalysis and Exploration Technology of Ministry of Natural Resources, Zhengzhou 450012, China | | TANG Yiqiu | Rock and Mineral Testing Center of Henan Province, Key Laboratory of Precious MetalsAnalysis and Exploration Technology of Ministry of Natural Resources, Zhengzhou 450012, China |
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| 中文摘要: |
| 以毒性小、不易挥发的氧化铋为贵金属捕集剂，硝酸银和亚碲酸钾(mAg/mTe)=1:1为灰吹保护剂，将铋扣在镁砂灰皿中820℃一次灰吹的留铋碲银珠，在预置少量硼砂的瓷坩埚中二次灰吹，得到光滑纯净的贵金属碲银合粒。合粒经王水高压密闭消解后，以Lu、In为内标，ICP-MS测定贵金属，Au、Pt、Pd在0.1~1000 ng/mL，Rh、Ir、Ru在0.1~500 ng/mL线性关系较好，r均大于0.9998。Au、Pt、Pd、Rh、Ir、Ru的方法检出限分别为0.24、0.22、0.21、0.017、0.018、0.019 ng/g，回收率均大于95%。对不同地区、不同类型标准物质测定，结果与认定值的相对标准偏差(RSD)均小于8.57%，相对误差(RE)为-10.00%~15.79%。 |
| 英文摘要: |
| In this work, lower toxic and less volatile bismuth oxide (Bi2O3) was used as the fire assay collector, and a mixture of AgNO3 and K2TeO3 (mAg/mTe=1:1) as the protection cupellation to generate Bi granule. Bi granule was put in magnesia cupel. After cupellated at 820℃, it was transferred into porcelain crucible for the secondary cupellation. Finally, smooth and pure precious metal tellurium silver granules was obtained. After Ag/Te granule was digested under high pressure by aqua regia, it was submitted for analysis by inductively coupled plasma mass spectrometry (ICP-MS) using Lu and In as internal standard. Under the optimal conditions, excellent curve fitting of Au/Pt/Pd and Rh/Ru/Ir was obtained between 0.1~1000 ng/mL and 0.1~500 ng/mL, respectively, with the correlation coefficients exceeding 0.9998. The detection limits of the method were 0.24, 0.22, 0.21, 0.017, 0.018, 0.019 ng/g, respectively, for Au, Pt, Pd, Rh, Ir and Ru, and the recoveries were higher than 95%. The developed method was applied to the analysis of the multi-types of certified reference materials. The relative standard deviation (RSD) between the results and the certified value was less than 8.57%, and the relative error (RE) was -10.00%~15.79%. |
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