ICP-OES法测定镍硼中硼、铁、硅及铝  

Determination of B,Fe,Si and Al in nickel boron alloy by ICP-OES

作　　者：李冀辉 李蒙 刘琴 刘丽静[5] LI Jihui;LI Meng;LIU Qin;LIU Lijing(Jiangxi University of Science and Technology,Ganzhou 330013,China;Inner Mongolia Rare Earth Ovonic Metal Hydride Co.,Ltd.,Baotou 014030,China;State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization,Baotou 014030,China;Baotou Research Institute of Rare Earths,Baotou 014030,China;Baotou Teachers College,Baotou 014030,China)

机构地区：[1]江西理工大学,江西赣州341000 [2]内蒙古稀奥科贮氢合金有限公司,内蒙古包头014030 [3]白云鄂博稀土资源研究与综合利用全国重点实验室,内蒙古包头014030 [4]包头稀土研究院,内蒙古包头014030 [5]包头师范学院,内蒙古包头014030

出　　处：《中国有色冶金》2025年第1期122-128,共7页China Nonferrous Metallurgy

基　　金：国家自然科学基金(22065028);内蒙古教育厅重点项目(NJzz23110);包头师范学院科研项目(BSYKJ2022-ZY02)。

摘　　要：镍硼合金中硼是主量元素,含量高低将直接影响合金的力学性能,合金中铁、硅及铝等元素也是重要的检测指标,现有的分析检测方法存在干扰元素影响大、操作步骤复杂且分析测定时间长等问题。本文建立了ICP-OES法测定镍硼合金中硼、铁、硅及铝含量的方法,对样品的溶解方法进行了探索,并通过共存元素干扰及空白实验选择各元素的最佳分析波长,得出以下主要结论。采用王水溶解+碱熔残渣方式分解试样,样品溶解完全,测定溶液盐分较低,各元素的测定下限可满足分析要求;在选定分析波长下对各元素进行检测,铁、硅及铝的检出限分别为0.009 0μg/mL、0.039μg/mL、0.018μg/mL;试验过程中硼、铁、硅及铝的回收率为88%~106%,实际样品测定的相对标准偏差(RSD,n=11)为0.54%~9.6%;同时使用实验方法和容量法、原子吸收光谱法、分光光度法及ICP-MS法测定硼镍合金中硼、铁、硅及铝量,测定结果基本一致。本研究方法可进行多元素同时测定,方法简便、快捷,测定结果准确、可靠,可作为检测镍硼合金主量及重要杂质元素含量指标的主要分析方法。The existing analysis methods have problems such as significant interference from elements,miscellaneous steps,and long time.The method was established to determine the content of B,Fe,Si and Al in nickel boron alloys by ICP-OES.We explored the dissolution method of the sample and selected the optimal wavelength for each element through coexisting element interference and blank experiments.The following main conclusions were drawn.The sample was decomposed using aqua regia dissolution and alkali melting residue method,and the sample was completely dissolved.The measured solution had low salt content,and the lower limit of each element could meet the analysis requirements.Detecting each element at the selected wavelength,the determination limit of Fe,Si and Al were 0.009 0 μg/mL,0.039 μg/mL and 0.018 μg/mL.According to the method,the recovery rates of B,Fe,Si and Al are 88% to 106%.The relative standard deviations(RSD,n=11) of actual sample were between 0.54% and 9.6%.Meanwhile the content of B,Fe,Si and Al in nickel boron alloys was also determined by volumetric method,atomic absorption spectroscopy,spectrophotometry and ICP-MS method,the results were basically consistent with those obtained by the experimental method.This research method can be used for simultaneous determination of multiple elements,which is simple,fast,accurate,and reliable.It can be used as the main analytical method for detecting the main content and important impurity element content indicators of nickel boron alloys.

关 键 词：镍硼合金 硼、铁、硅、铝测定 ICP-OES法 样品分解 王水溶解+碱熔残渣 干扰元素 分析波长 

分 类 号：O657.31[理学—分析化学] TF125[理学—化学]