电感耦合等离子体原子发射光谱(ICP-AES)法测定真空精炼镁合金物料中铁、铜、镍  

Determination of Iron,Copper and Nickel in Vacuum Refined Magnesium Alloy Materials by Inductively Coupled Plasma Atomic Emission Spectrometry

作　　者：孙洪飞 王立鹏 李蕊[1,2,3,4] 唐飞龙 杨柒梅 伍秋云 田阳 吴鉴[1,2,3,4] SUN Hongfei;WANG Lipeng;LI Rui;TANG Feilong;YANG Qimei;WU Qiuyun;TIAN Yang;WU Jian(Key Laboratory for Nonferrous Vacuum Metallurgy of Yunnan Province,Kunming University of Science and Technology,Kunming,Yunnan 650093,China;State Key Laboratory of Complex Non-ferrous Metal Resources Clean Utilization,Kunming University of Science and Technology,Kunming,Yunnan 650093,China;National Engineering Research Center of Vacuum Metallurgy,Kunming University of Science and Technology,Kunming,Yunnan 650093,China;Faculty of Metallurgical and Energy Engineering,Kunming University of Science and Technology,Kunming,Yunnan 650093,China)

机构地区：[1]昆明理工大学云南省有色金属真空冶金重点实验室,昆明650093 [2]昆明理工大学省部共建复杂有色金属资源清洁利用国家重点实验室,昆明650093 [3]昆明理工大学真空冶金国家工程研究中心,昆明650093 [4]昆明理工大学冶金与能源工程学院,昆明650093

出　　处：《中国无机分析化学》2024年第4期464-472,共9页Chinese Journal of Inorganic Analytical Chemistry

基　　金：云南省科技厅重大科技专项研究基金资助项目(202302AB080002);云南省有色金属真空冶金顶尖团队(202305AS350012)。

摘　　要：真空精炼是目前镁金属提纯的重要工艺,工艺原料及真空精炼提纯镁金属过程残留物中Fe、Cu、Ni含量的准确测定对工艺参数的优化及调整具有重要的指导作用。传统测定方法中以邻二氮杂菲分光光度法、新亚铜灵分光光度法、丁二酮肟分光光度法测定三种元素含量,结果准确,但操作繁琐,周期较长,难以满足工业生产中高效、快速测定的需要,且方法中所需的有机萃取剂对环境污染较大。选择电感耦合等离子体发射光谱(ICP-AES)法测定真空蒸馏精炼镁合金物料中Fe、Cu、Ni,系统探究溶解酸、溶解温度、溶解时间对物料溶解和测定的影响,选择盐酸(1+1)和过氧化氢溶解体系,200℃加热条件下反应20 min为最佳消解镁合金原料条件;选择王水溶解体系,200℃加热条件下反应25 min为真空精炼残留物最佳溶解条件。并探讨ICP-AES测定过程中各元素的检出限和测定下限以及共存元素的干扰情况,建立了ICP-AES法测定真空精炼提纯镁合金物料的方法。测定结果的相对标准偏差(RSD,n=11)为Fe 5.9%~11.5%、Cu 2.6%~11.8%、Ni 3.4%~11.5%,各元素加标回收率为Fe 96.4%~102%、Cu 101%~108%、Ni 103%~105%;按照建立的方法测定镁合金原料、真空精炼残留物中的铁、铜、镍,并与国家标准方法测定结果进行对比,结果相一致。实现了ICP-AES法快速、准确测定真空蒸馏精炼镁合金物料中铁、铜、镍含量,对及时、高效、准确评估真空精炼提纯镁工艺及产品具有重要意义。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 contents 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 20 min reaction at 200℃.The solution system of aqua regia was selected,and 25 min reaction at 200℃was the optimum 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(RSD,n=11)were Fe 5.9%-11.5%,Cu 2.6%-11.8%,and Ni 3.4%-11.5%.The recoveries of each element were Fe 96.4%-102%,Cu 101%-108%,and Ni 103%-105%.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

关 键 词：电感耦合等离子体发射光谱法(ICP-AES) 真空精炼 残留物 铁 铜 镍 

分 类 号：O657.31[理学—分析化学]