电感耦合等离子体原子发射光谱(ICP-AES)法测定铝铍中间合金中的铍
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摘要
通过对铍的自吸效应和光谱干扰研究,选取了Be(Ⅱ)313.1nm作为分析线,建立了铝铍合金中测定铍元素含量的电感耦合等离子体原子发射光谱(ICP-AES)法。实验结果表明,谱线Be(Ⅱ)313.0nm的线性范围达到20μg/mL,谱线Be(Ⅱ)3 131nm的线性范围可达30μg/mL,当溶液中铍元素的浓度超过线性范围时,两条谱线的工作曲线发生弯曲,产生明显的自吸效应,样品分析过程中避免使用有自吸效应的谱线,可以大大提高分析结果的准确性;样品中主要杂质元素和基体对铍的谱线不产生光谱干扰。方法中铍的检出限为0.000 4%。铍的质量浓度在1.0~15μg/mL时,工作曲线的线性回归方程为y=265.101 0x+0.45,相关系数R=0.999 645。按实验方法分别对铝铍合金样品和合成的模拟标准样品进行回收率和精密度实验,标准加入回收率在101%~103%,相对标准偏差在0.58%~0.98%。方法能够准确快速地分析铝铍中间合金中铍的含量。
In this paper,a method for determination of beryllium(Be)in aluminum-beryllium alloys was established by inductively coupled plasma-atomic emission spectrometry(ICP-AES).Linear calibration was achieved up to the range of 20μg/mL using Be(II)313.0 nm line whileusing Be(Ⅱ)313.1 nm line,calibration up to 30μg/mL was obtained.For higher Be mass concentrations,self-absorption resulted in non-linearity of calibration curve which can be avoided by selecting lines free from self-absorption.Moreover,selected Be lines were free from spectral interference of coexisting elements in the matrix.The Be limit of detection by the present method was determined 0.0004%(mass fraction).For Be concentration range of 1.0~15μg/mL,linear regression of working curve was y =265.101 0 x+0.45 with correlationcoefficient of R =0.999 645.The recovery rates were between 101% ~104% and the relative standard deviation resides between 0.58% ~0.98%.The present results showed that the present method can be used for accurate and fast determination of Be concentration in aluminum-beryllium alloys.
In this paper,a method for determination of beryllium(Be)in aluminum-beryllium alloys was established by inductively coupled plasma-atomic emission spectrometry(ICP-AES).Linear calibration was achieved up to the range of 20μg/mL using Be(II)313.0 nm line whileusing Be(Ⅱ)313.1 nm line,calibration up to 30μg/mL was obtained.For higher Be mass concentrations,self-absorption resulted in non-linearity of calibration curve which can be avoided by selecting lines free from self-absorption.Moreover,selected Be lines were free from spectral interference of coexisting elements in the matrix.The Be limit of detection by the present method was determined 0.0004%(mass fraction).For Be concentration range of 1.0~15μg/mL,linear regression of working curve was y =265.101 0 x+0.45 with correlationcoefficient of R =0.999 645.The recovery rates were between 101% ~104% and the relative standard deviation resides between 0.58% ~0.98%.The present results showed that the present method can be used for accurate and fast determination of Be concentration in aluminum-beryllium alloys.
引文
[1]刘孝宁,马世光.铍铝合金的研究与应用[J].稀有金属(Chinese Journal of Rare Metals),2003,27(1):62-65.
[2]崔爽,周兵,赵世卓.ICP-AES光谱法测定铝-铍中间合金各元素含量[J].中小企业管理与科技(Management and Technology of SME),2011(21):297.
[3]谢奕斌,温亚勇,孙秀娟.电感耦合等离子体原子发射光谱法测定铍铝合金中的铍、铁、锰、硅[J].精细化工中间体(Fine Chemical Intermediates),2011,41(1):70-72.
[4]王强,叶晓英,李刚,等.电感耦合等离子体原子发射光谱法测定铝合金中铍[J].冶金分析(Metallurgical Analysis),2015,35(12):51-54.
[5]孙洪涛,李淑兰,邓培,等.ICP-AES法测定铍铜合金中Be,Ni,Ti,Co,Fe,Al,Si,Mg和Pb[J].稀有金属(Chinese Journal of Rare Metals),2003,27(6):857-859.
[6]孙洪涛,杨娟,侯学娟.金属材料中铍分析方法的综述[J].广州化工(Guangzhou Chemical Industry),2017,45(2):25-27.
[7]D.Sc.蒂博尔托罗克.发射光谱化学分析[M].黄存礼译.长沙:中南工业大学出版社,1978:169-170.
[8]AHRENS LH.分光化学分析[M].殷万,译.北京:地质出版社,1956:120-123.
[9]李天生,王鸿辉,潘忠厚.高钼材料的ICP-AES分析和基体效应及自吸效应的研究Ⅱ.钼铁中主、微量元素分析和自吸效应研究[J].现代商检科技(Modern Commodity Inspection Science and Technique),1994,4(2):8-13.
[10]HUMAN H G C,SCOTT R H.The shapes of spectral lines emitted by aninductively coupled plasma[J].Spectrochimica Acta,1976(31B):459-473.
[2]崔爽,周兵,赵世卓.ICP-AES光谱法测定铝-铍中间合金各元素含量[J].中小企业管理与科技(Management and Technology of SME),2011(21):297.
[3]谢奕斌,温亚勇,孙秀娟.电感耦合等离子体原子发射光谱法测定铍铝合金中的铍、铁、锰、硅[J].精细化工中间体(Fine Chemical Intermediates),2011,41(1):70-72.
[4]王强,叶晓英,李刚,等.电感耦合等离子体原子发射光谱法测定铝合金中铍[J].冶金分析(Metallurgical Analysis),2015,35(12):51-54.
[5]孙洪涛,李淑兰,邓培,等.ICP-AES法测定铍铜合金中Be,Ni,Ti,Co,Fe,Al,Si,Mg和Pb[J].稀有金属(Chinese Journal of Rare Metals),2003,27(6):857-859.
[6]孙洪涛,杨娟,侯学娟.金属材料中铍分析方法的综述[J].广州化工(Guangzhou Chemical Industry),2017,45(2):25-27.
[7]D.Sc.蒂博尔托罗克.发射光谱化学分析[M].黄存礼译.长沙:中南工业大学出版社,1978:169-170.
[8]AHRENS LH.分光化学分析[M].殷万,译.北京:地质出版社,1956:120-123.
[9]李天生,王鸿辉,潘忠厚.高钼材料的ICP-AES分析和基体效应及自吸效应的研究Ⅱ.钼铁中主、微量元素分析和自吸效应研究[J].现代商检科技(Modern Commodity Inspection Science and Technique),1994,4(2):8-13.
[10]HUMAN H G C,SCOTT R H.The shapes of spectral lines emitted by aninductively coupled plasma[J].Spectrochimica Acta,1976(31B):459-473.