电感耦合等离子体原子发射光谱法测定钼铌合金中8种元素
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摘要
采用5.0 mL氢氟酸和10.0 mL硝酸混合酸消解样品,选择Ce 407.570nm、Cu217.895nm、Fe 234.350nm、Er 390.631nm、Mg 383.829nm、Mn 257.610nm、Pb 283.305nm、Zn 213.857nm为分析线,使用电感耦合等离子体原子发射光谱法(ICP-AES)进行测定,从而建立了电感耦合等离子体原子发射光谱法测定钼铌合金中Ce、Cu、Fe、Er、Mg、Mn、Pb、Zn等8种元素的分析方法。考察了主要元素Mo、Nb和Al对待测元素的影响,结果表明,这些元素对待测元素基本无影响。各元素校准曲线的线性相关系数均大于0.999;方法中各元素检出限为5.4~63μg/g。按照实验方法测定钼铌合金样品中Ce、Cu、Fe、Er、Mg、Mn、Pb、Zn,结果的相对标准偏差(RSD,n=6)为0.89%~4.4%;回收率为98%~102%。按照实验方法测定钼铌合金样品中Cu、Fe、Er、Mg、Mn、Pb、Zn、Ce,并与电感耦合等离子体质谱法(ICPMS)的测定结果进行比对,二者基本一致。
The sample was digested with the mixed acid combined with 5.0mL of hydrofluoric acid and 10.0mL of nitric acid.Ce 407.570 nm,Cu 217.895 nm,Fe 234.350 nm,Er 390.631 nm,Mg 383.829 nm,Mn257.610 nm,Pb 283.305 nm and Zn 213.857 nm were selected as analytical lines.Consequently,an analysis method of eight elements(including Ce,Cu,Fe,Er,Mg,Mn,Pb and Zn)in molybdenum-niobium alloy by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.The influence of major elements(Mo,Nb and Al)on test elements was investigated.The results indicated that these elements had no significant influence on determination.The linear correlation coefficients of calibration curves were all higher than 0.999.The detection limits of elements were between 5.4μg/g and 63μg/g.The proposed method was applied for the determination of Ce,Cu,Fe,Er,Mg,Mn,Pb and Zn in molybdenum-niobium alloy samples.The relative standard deviations(RSD,n=6)were between 0.89% and4.4%.The recoveries were between 98% and 102%.The content of Ce,Cu,Fe,Er,Mg,Mn,Pb and Zn in molybdenum-niobium alloy samples was determined according to the experimental method.The results were consistent with those obtained by inductively coupled plasma mass spectrometry(ICP-MS).
The sample was digested with the mixed acid combined with 5.0mL of hydrofluoric acid and 10.0mL of nitric acid.Ce 407.570 nm,Cu 217.895 nm,Fe 234.350 nm,Er 390.631 nm,Mg 383.829 nm,Mn257.610 nm,Pb 283.305 nm and Zn 213.857 nm were selected as analytical lines.Consequently,an analysis method of eight elements(including Ce,Cu,Fe,Er,Mg,Mn,Pb and Zn)in molybdenum-niobium alloy by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.The influence of major elements(Mo,Nb and Al)on test elements was investigated.The results indicated that these elements had no significant influence on determination.The linear correlation coefficients of calibration curves were all higher than 0.999.The detection limits of elements were between 5.4μg/g and 63μg/g.The proposed method was applied for the determination of Ce,Cu,Fe,Er,Mg,Mn,Pb and Zn in molybdenum-niobium alloy samples.The relative standard deviations(RSD,n=6)were between 0.89% and4.4%.The recoveries were between 98% and 102%.The content of Ce,Cu,Fe,Er,Mg,Mn,Pb and Zn in molybdenum-niobium alloy samples was determined according to the experimental method.The results were consistent with those obtained by inductively coupled plasma mass spectrometry(ICP-MS).
引文
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[16]龚思维,楚民生,沈泽敏,等.ICP-AES法测定铝中铁、硅、铜、镓、镁、锌、锰和钛[J].分析试验室,2004,23(1):40-42.GONG Si-wei,CHU Min-sheng,SHEN Ze-min,et al.Determination of Fe,Si,Cu,Ga,Mg,Zn,Mn,Ti in aluminum by ICP-AES[J].Chinese Journal of Analysis Laboratory,2004,23(1):40-42.
[2]Zee R H,Xiao Z,Chin B A,et al.Processing of single crystals for high temperature applications[J].Journals of Materials Processing Technology,2001,113:75-80.
[3]张忠士.一种铝钼铌硅中间合金及其制备方法:中国,CN1629342[P].2005-06-22.
[4]邓秀琴,高辉.钼蓝光度法快速测定钼铁中的硅[J].化学分析计量,2008,17(4):56-57.DENG Xiu-qin,GAO Hui.Rapid determination of silicon in ferromolybdenum alloy with molybdenum blue by spectrophotometry[J].Chemical Analysis and Meterage,2008,17(4):56-57.
[5]邱少花,张东雯,任娟玲.原子荧光法测定焙烧钼精矿及钼铁中的锑[J].中国钼业,2015,39(2):37-40.QIU Shao-hua,ZHANG Dong-wen,REN Juan-ling.An atomic fluorescent method for the determination of antimony in the roasted molybdenum concentrate and ferromolybdenum[J].China Molybdenum Industry,2015,39(2):37-40.
[6]李波,周恺,孙宝莲,等.X射线荧光光谱法测定钼铝合金中钼[J].冶金分析,2013,33(9):42-45.LI Bo,ZHOU Kai,SUN Bao-lian,et al.Determination of molybdenum in molybdenum-aluminum alloy by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2013,33(9):42-45.
[7]马琪,蒙娟娟.电感耦合等离子体原子发射光谱法测定钼铜合金中镍、钙、镁、铝含量[J].理化检验:化学分册,2012(12):1496-1497.MA Qi,MENG Juan-juan.Determination of Ni,Ca,Mg,Al in Mo-Cu alloy by ICP-AES[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2012(12):1496-1497.
[8]禄妮,李波,石新层,等.ICP-AES法测定钼合金中的镧元素[J].稀有金属快报,2007(2):40-42.LU Ni,LI Bo,SHI Xin-ceng,et al.Determination of La in molybdenum alloy by ICP-AES[J].Rare Metals Letters,2007(2):40-42.
[9]成勇,肖军,宁燕平,等.ICP-AES法测定钼铁中Mo,Si,Cu,Sb,Sn[J].冶金分析,2003,23(3):28-30.CHENG Yong,XIAO Jun,NING Yan-ping,et al.Simultaneous determination of Mo,Si,Cu,Sb and Sn in Mo-Fe alloy by ICP-AES[J].Metallurgical Analysis,2003,23(3):28-30.
[10]辛仁轩.等离子体发射光谱分析[M].北京:化学工业出版社,2005:140-144.
[11]刘婷,李剑,雷小燕,等.ICP-AES法测定70Ni-30Mo镍钼中间合金中钼、铁、铝、硅、磷[J].化学分析计量,2014,24(4):72-74.LIU Ting,LI Jian,LEI Xiao-yan,et al.Determination of Mo,Fe,Al,Si,P,in 70Ni-30Mo Nickel-molybdenum alloy by ICP-AES[J].Chemical Analysis and Meterage,2014,24(4):72-74.
[12]杨小刚,杜昕,姚亮.ICP-AES技术应用的研究进展[J].现代科学仪器,2012(3):139-144.YANG Xiao-gang,DU Xin,YAO Liang.Progresses of application and research for ICP-AES technology[J].Modern Scientific Instruments,2012(3):139-144.
[13]辛仁轩,余正东,郑建明,等.电感耦合等离子体原子发射光谱法原理及应用[M].北京:冶金工业出版社,2012:199.
[14]侯列奇,王树安,李洁,等.电感耦合等离子体原子发射光谱法测定铀-钼合金中15种微量杂质元素[J].理化检验:化学分册,2007,43(3):179-181.HOU Lie-qi,WANG Shu-an,LI Jie,et al.Determination of micro-amounts of 15elements present as impurities in uranium-molybdenum alloy[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2007,43(3):179-181.
[15]张颖.阳离子交换ICP-OES测定高纯氧化铌中十三种杂质元素[J].硬质合金,2006,23(3):147-149.ZHANG Ying.Determination of 13impurities in highpurity niobium pentoxide by cation exchange ICP-OES[J].Cemented Carbide,2006,23(3):147-149.
[16]龚思维,楚民生,沈泽敏,等.ICP-AES法测定铝中铁、硅、铜、镓、镁、锌、锰和钛[J].分析试验室,2004,23(1):40-42.GONG Si-wei,CHU Min-sheng,SHEN Ze-min,et al.Determination of Fe,Si,Cu,Ga,Mg,Zn,Mn,Ti in aluminum by ICP-AES[J].Chinese Journal of Analysis Laboratory,2004,23(1):40-42.