摘要
在锑铍芯块中,锑的质量分数为80%左右,铍的质量分数为20%左右。铍的存在会干扰电感耦合等离子体原子发射光谱法(ICP-AES)测定铁、镁、锰、铅、铝,另外锑的水解也会影响测定。试验使用盐酸、硝酸和酒石酸处理样品,选择Fe 240.488nm、Mg 285.213nm、Mn259.373nm、Pb 182.205nm、Al 308.215nm作为分析谱线,采用标准加入法(MSA)绘制校准曲线可消除铍、锑基体效应的影响,酒石酸也可完全抑制锑的水解,使用ICP-AES测定铁、镁、锰、铅、铝,从而建立了锑铍芯块中铁、镁、锰、铅、铝等杂质元素的分析方法。各元素在10~400μg/g范围内,校准曲线的线性相关系数均大于0.9998;方法中各元素的检出限为0.48~3.6μg/g。实验方法用于测定2个铍锑芯块样品中铁、铅、镁、锰、铝,结果的相对标准偏差(RSD,n=11)为1.1%~4.9%。按照实验方法和其他方法(铁、铅、镁、锰采用原子吸收光谱法,铝使用分光光度法)测定2个锑铍芯块样品中铁、铅、镁、锰、铝,测定结果相一致。
In antimony-beryllium pellet,the mass fraction of antimony is about 80%and that of beryllium is about 20%.The presence of beryllium will affect the determination of iron,magnesium,manganese,lead and aluminum by inductively coupled plasma atomic emission spectrometry(ICP-AES).Moreover,the hydrolysis of antimony will also affect the determination.The samples were treated with hydrochloric acid,nitric acid and tartaric acid.Fe 240.488 nm,Mg 285.213 nm,Mn 259.373 nm,Pb 182.205 nm and Al 308.215 nm were selected as the analytical lines.The preparation of calibration curves by the method of standard addition(MSA)could eliminate the influence of matrix effect caused by beryllium and antimony.Moreover,the hydrolysis of antimony could be completely inhibited using tartaric acid.The content of iron,magnesium,manganese,lead and aluminum were determined by ICP-AES.Consequently the analysis method of impurities in antimony-beryllium pellet such as iron,magnesium,manganese,lead and aluminum was established.When the contents of elements were in range of 10-400μg/g,the linear correlation coefficients of calibration curves were all higher than 0.9998.The detection limits of elements in this method were between 0.48 and 3.6μg/g.The proposed method was applied for the determination of iron,magnesium,manganese,lead and aluminum in two antimony-beryllium pellet samples.The relative standard deviations(RSD,n=11)of the results were between 1.1%and 4.9%.The contents of iron,magnesium,manganese,lead and aluminum in two antimony-beryllium pellet samples were determined according to the experimental method and other methods(atomic absorption spectrometry for iron,lead,magnesium and manganese,and spectrophotometry for aluminum),and the results were consistent.
作者
王志萍
殷艺丹
WANG Zhi-ping;YIN Yi-dan(State Key Laboratory of Rare Metal Special Materials,Northwest Rare Metal Materials Research Institute Ningxia Co.,Ltd.,Shizuishan 75300,China)
出处
《冶金分析》
CAS
北大核心
2019年第11期79-83,共5页
Metallurgical Analysis
关键词
电感耦合等离子体原子发射光谱法
锑铍芯块
铁
镁
锰
铅
铝
标准加入法
inductively coupled plasma atomic emission spectrometry
antimony-beryllium pellet
iron
magnesium
manganese
lead
aluminum
method of standard addition
作者简介
王志萍(1972—),女,高级工程师,大学本科,主要从事光谱分析测试与研究;E-mail:gonggd@cnmnc.com。
