Determination of arsenic, tin, antimony and bismuth inferromolybdenum by hydride generation-inductivelycoupled plasma atomic emission spectrometry
YANG Li-feng, LIU Guo-jun*, WU Zhi-hong, WANG Jian-xin, MIAO Ji-wei, LIU Ying-yang
Inner Mongolia Autonomous Region Key Laboratory of Testing and Testing Technology for Special Steel andIts Products, Measurement and Testing Technology Institute, Inner Mongolia North Heavy Industries GroupCorp., Ltd., Baotou 014033, China
Abstract：Ferromolybdenum is used as the additive of molybdenum in smelting process. In order to ensure the quality of smelting, the contents of arsenic, tin, antimony and bismuth should be strictly controlled. The national standard or atomic fluorescence spectrometry can only detect the single element. Moreover, the analysis speed is slow and the analysis period is long. Arsenic, tin, antimony and bismuth were reduced to volatile covalent hydrides in an acid reduction system containing 0.264mol/L sodium borohydride and 40% hydrochloric acid. Then the produced volatile covalent hydrides were introduced to inductively coupled plasma optical emission spectrometer by carrier gas for measurement. Consequently the determination method of arsenic, tin, antimony and bismuth in ferromolybdenum by hydride generation-inductively coupled plasma optical emission spectrometry (ICP-AES) was established. As 193.759nm, Sn 189.989nm, Sb 217.581nm and Bi 223.061nm were selected as the analytical lines for elements. In order to eliminate the influence of matrix effect, the standard solution series were prepared by matrix matching method to draw the calibration curve. The linear correlation coefficients of calibration curves of elements were higher than 0.999. The limit of detection for arsenic, tin, antimony and bismuth was 0.0003%, 0.0009%, 0.0009% and 0.0012%, respectively. The proposed method was applied for the determination of arsenic, tin, antimony and bismuth in ferromolybdenum sample. The relative standard deviations (RSD, n=6) of measurements results were between 3.1% and 4.8%. The spiked recoveries were between 92% and 110%.
支国瑞,刘吉红,卢艳军,等.ICP-AES 测定钼铁中微量锑和锡[J].理化检验:化学分册,2002,38(9):459-461.ZHI Guo-rui,LIU Ji-hong,LU Yan-jun,et al.ICP-AES Determination of micro amounts of antimony and tin in ferromolybdenum[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2002,38(9):459-461.
官东超,赵平涛.ICP-AES同时测定锡多金属矿中锡钨钼铁铜铅锌砷锑[J].华东科技:学术版(East China Science & Technology),2017(9):5.
[7]
侯列奇,李洁.电感耦合等离子体原子发射光谱法测定金属钼中10种微量元素[J].理化检验:化学分册,2009,45(2):148-150.HOU Lie-qi,LI Jie.Determination of elements of microamounts in molybdenum metal by inductively coupled plasma atomic emission spectrometry[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2009,45(2):148-150.
[8]
邓传东,孙琳,安身平,等.电感耦合等离子体原子发射光谱(ICP-AES)法测定南红玛瑙中剧毒元素As,Cd,Cr,Pb,Sb的含量[J].中国无机分析化学,2018,8(6):9-13.DENG Chuan-dong,SUN Lin,AN Shen-ping,et al.Determination of toxic elements As,Cd,Cr,Pb,Sb in southern red agate by ICP-AES[J].Chinese Jorunal of Inorganic Analytical Chemistry,2018,8(6):9-13.
[9]
罗治定,陈庆芝,金倩,等.预还原氢化物发生-原子荧光光谱法快速测定化探样品中的As,Sb,Bi,Hg[J].中国无机分析化学,2018,8(2):17-21.LUO Zhi-ding,CHEN Qing-zhi,JIN Qian,et al.Quick determination of As,Sb,Bi,Hg in geochemical samples by prereduction hydride generation-atomic fluorescence spectrometry[J].Chinese Jorunal of Inorganic Analytical Chemistry,2018,8(2):17-21.
[10]
张巨成,曾宪津,张卓勇.氢化物发生-ICP-AES法同时测定铅及其他氢化物及非氢化物元素[J].光谱学与光谱分析,1990,10(5):36-40.ZHANG Ju-cheng,ZENG Xian-jin,ZHANG Zhuo-yong.Simultaneous determination of lead,arsenic,antimony,bismuth,tin,germanium and nonhydride-forming elements by ICP-AES with a modified cyclone nebulizer-hydride generator[J].Spectroscopy and Spectral Analysis,1990,10(5):36-40.
[11]
连小安,周扬杰.氢化物发生-原子荧光光谱法同时测定钼铁中的锑和锡含量[J].铁合金,2018(3):40-43.LIAN Xiao-an,ZHOU Yang-jie.Simultaneous determination of antimony and tin in ferromolybdenum by hydride generation atomic fluorescence spectrometry method[J].Ferro-Alloys,2018(3):40-43.
[12]
Ilander A,Väisänen A. The determination of antimony and arsenic concentrations in fly ash by hydride generation inductively coupled plasma optical emission spectrometry[J].Analytica Chimica Acta,2011(2):178-183.
[13]
Nereida Carrión,Miguel Murillo,Edie Montiel,et al.Development of a direct hydride generation nebulizer for the determination of selenium by inductively coupled plasma optical emission spectrometry[J].Spectrochimica Acta Part B:Atomic Spectroscopy,2003,58(8):1375-1389.
