电感耦合等离子体原子发射光谱法测定核级铁铬铝合金中10种杂质元素  

Determination of ten impurity elements in nuclear grade ironchromium-aluminum alloy by inductively coupled plasma atomic emission spectrometry

作　　者：杨平[1] 邓传东 孙琳 盛红伍[1] 安身平[1] YANG Ping;DENG Chuan-dong;SUN Lin;SHENG Hong-wu;AN Shen-ping(State Key Laboratory for Reactor Fuel and Materials,Nuclear Power Institute of China,Chengdu 610213,China)

机构地区：[1]中国核动力研究设计院反应堆燃料及材料国家重点实验室

出　　处：《冶金分析》2019年第11期74-78,共5页Metallurgical Analysis

摘　　要：核级铁铬铝合金是非常重要的包壳材料,杂质元素含量对其性质有着十分重要的影响,因此需要准确测定其含量。采用硝酸-盐酸混合酸溶解,再加氢氟酸使样品完全溶解。选择Mn 257.610nm、Mo 204.598nm、Nb 295.088nm、Ni 231.604nm、Si 212.412nm、Ta269.452nm、Ti 334.941nm、V 310.230nm、Y 371.030nm、Zr 327.305nm作为分析谱线,采用基体匹配法绘制校准曲线消除基体效应的影响,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定核级FeCrAl合金中Mn、Mo、Nb、Ni、Si、Ta、Ti、V、Y、Zr等10种杂质元素含量的方法。各元素在线性范围内,校准曲线线性相关系数均不小于0.9997;方法中各元素检出限为0.30~31μg/g。按照实验方法测定核级FeCrAl合金中10种杂质元素,结果的相对标准偏差(RSD,n=6)为1.1%~4.5%,加标回收率为95%~105%。Nuclear grade Fe-Cr-Al alloy is a very important cladding material.The content of impurity elements in nuclear grade Fe-Cr-Al alloy is critical to its properties and should be accurately determined.The sample was dissolved with nitric acid-hydrochloric acid mixture.Then hydrofluoric acid was added to completely dissolve the sample.Mn 257.610 nm,Mo 204.598 nm,Nb 295.088 nm,Ni 231.604 nm,Si 212.412 nm,Ta 269.452 nm,Ti 334.941 nm,V 310.230 nm,Y 371.030 nm,Zr 327.305 nm were selected as the analytical spectral lines.The calibration curve was prepared by matrix matching method to eliminate the matrix effect.Consequently the determination method of ten impurity elements(including Mn,Mo,Nb,Ni,Si,Ta,Ti,V,Y and Zr)in nuclear grade iron-chromium-aluminum alloy by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.Within the linear ranges of each element,the correlation coefficients of calibration curves were all greater than 0.9997.The detection limits of elements in this method were in the range of 0.30-31μg/g.Ten impurity elements in nuclear grade iron-chromium-aluminum alloy were determined according to the experimental method.The relative standard deviations(RSD,n=6)were between 1.1%and 4.5%.The spiked recoveries were between 95%and 105%.

关 键 词：核级铁铬铝合金 电感耦合等离子体原子发射光谱法(ICP-AES) 锰 钼 铌 镍 硅 钽 钛 钒 钇 锆 

分 类 号：O657.31[理学—分析化学] TF031[理学—化学]