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| Determination of iron, copper and nickel in vacuum refined magnesium alloy materials by inductively coupled plasma emission spectrometry |
| Received:June 26, 2023 Revised:December 26, 2023 |
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| DOI：10.3969/j.issn.2095-1035.2024.04.012 |
| KeyWord:Inductively coupled plasma emission spectrometry (ICP-AES); Vacuum refining; Residue; Iron; Copper; nickel. |
| Author | Institution |
| sunhongfei |
昆明理工大学 |
| Wanglipeng |
昆明理工大学 |
| LiRui |
昆明理工大学 |
| TangFeiLong |
昆明理工大学 |
| YangQiMei |
昆明理工大学 |
| WuQiuYun |
昆明理工大学 |
| TianYang |
昆明理工大学 |
| WuJian |
昆明理工大学 |
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| Abstract: |
| Vacuum refining is an important process for magnesium metal purification at present. The accurate determination of Fe, Cu and Ni contents in raw materials and residues during vacuum refining has an important guiding effect on the optimization and adjustment of process parameters. In the traditional determination methods, o-diazazene spectrophotometry, neocuprine spectrophotometry and butanedione oxime spectrophotometry are used to determine the content of three elements. The results are accurate, but the operation is complicated and the cycle is long. It is difficult to meet the needs of efficient and rapid determination in industrial production, and the organic extraction agent required in the method causes great pollution to the environment. In this study, inductively coupled plasma emission spectrometry (ICP-AES) was used to determine Fe, Cu and Ni in vacuum distillation refined magnesium alloy materials. The influences of dissolved acid, dissolved temperature and dissolved time on material dissolution and determination were systematically explored. The dissolution system of (1+1) hydrochloric acid and hydrogen peroxide was selected. The optimal digestion condition of magnesium alloy raw material was 20min reaction at 200℃. The solution system of aqua regia was selected, and 25min reaction at 200℃ was the best solution condition for vacuum refining residue. The detection limit and limit of each element in the determination process of ICP-AES and the interference of co-existing elements were discussed. The relative standard deviations (RSDS, n=11) were Fe 5.89% ~ 11.49%, Cu 2.58% ~ 11.78%, Ni 3.36% ~ 11.47%. The recovery rate of each element was; Fe 96.35% ~ 102%, Cu 101.3% ~ 108%, Ni 103% ~ 104.7%; The iron, copper and nickel in magnesium alloy raw material and vacuum refining residue were determined by the experimental method, and the results were compared with the national standard method. The rapid and accurate determination of Fe, Cu and Ni contents in vacuum distillation refined magnesium alloy materials by ICP-AES method was realized in this study, which is of great significance for timely, efficient and accurate evaluation of vacuum refining process and products of magnesium. |
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