Abstract：The all-vanadium redox flow battery was a widely used new energy technology. The solid vanadyl sulfate (VOSO4·nH2O, n=3-5) was the basic raw material for preparing vanadium electrolyte, and the content of vanadium and sulfate as well as their proportional relationship determined the quality of electrolyte and even vanadium battery. Therefore, the determination method of vanadium and sulfate in vanadyl sulfate for vanadium battery by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The analytical lines of testing elements with appropriate sensitivity were optimized and selected, which could meet the requirements for the simultaneous determination of vanadium and sulfate in vanadyl sulfate for vanadium battery with large content scope change. Moreover, the instrumental conditions such as integral region of analytical lines and the region of synchronous background correction were optimized to improve the detection performance of this method. The calibration curve was drawn with a series of mixed standard solutions containing vanadium and sulfate to eliminate the influence of matrix effect with matrix matching. The detection range for vanadium and sulfate was 15.0%-30.0% and 35.0%-50.0%, respectively. The linear correlation coefficients of calibration curves were all greater than 0.9999. The experimental method was applied for the determination of vanadium and sulfate in two vanadyl sulfate samples. The relative standard deviations (RSD, n=11) of results were less than 0.50%, and the recoveries were between 96% and 104%. The contents of vanadium and sulfate in three vanadyl sulfate samples were determined according the experimental method, and the results were compared with those obtained by ammonium persulfate oxidation-ammonium ferrous sulfate titration for vanadium and barium sulfate gravimetry for sulfate. The determination results were all in good agreement.
杨新能,冯宗平,羊绍松.电感耦合等离子体原子发射光谱法测定钒铁合金中杂质元素[J].冶金分析,2014,34(11):37-41.YANG Xin-neng,FENG Zong-ping,YANG Shao-song.Determination of impurity elements in ferrovanadium alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(11):37-41.
[2]
成勇,敬守斌.电感耦合等离子体原子发射光谱法测定钒铝合金中15种杂质元素[J].理化检验:化学分册,2013,49(1):44-47.CHENG Yong,JING Shou-bin.ICP-AES determination of 15 impurity elements in V-Al alloy[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(1):44-47.
[3]
冯宗平.电感耦合等离子体原子发射光谱法测定氧化钒中钾钠硫磷铁[J].冶金分析,2010,30(3):30-33.FENG Zong-ping.Determination of potassium,sodium,phosphorus,sulfur and iron in vanadium oxide by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2010,30(3):30-33.
[4]
周西林,王娇娜,刘迪,等.电感耦合等离子体原子发射光谱法在金属材料分析应用技术方面的进展[J].冶金分析,2017,37(1):39-46.ZHOU Xi-lin,WANG Jiao-na,LIU Di,et al.Inductively coupled plasma atomic emission spectrometry metal material application technology progress[J].Metallurgical Analysis,2017,37(1):39-46.
[5]
郑国经.电感耦合等离子体原子发射光谱分析仪器与方法的新进展[J].冶金分析,2014,34(11):1-10.ZHENG Guo-jing.New advances in inductively coupled plasma atomic emission spectrometries instruments and methods[J].Metallurgical Analysis,2014,34(11):1-10.
[6]
李玉忠,李建军.电感耦合等离子体原子发射光谱法测定硅铝钡钙系列合金主元素[J].冶金分析,2013,33(8):72-75.LI Yu-zhong,LI Jian-jun.Determination of main elements in Si-Al-Ba-Ca series alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2013,33(8):72-75.
[7]
胡璇,李跃平,石磊.基体匹配法和内标法-电感耦合等离子体原子发射光谱测定铸造锌合金中高含量铝和铜的光谱干扰校正的比较[J].冶金分析,2014,34(4):17-20.HU Xuan,LI Yue-ping,SHI Lei.Comparison on the spectral interference correction in the determination of high content of aluminum and copper in casting zinc alloy by inductively coupled plasma atomic emission spectrometry with matrix matching method and internal standard method[J].Metallurgical Analysis,2014,34(4):17-20.
[8]
成勇.电感耦合等离子体原子发射光谱法测定铌铁合金中铌[J].冶金分析,2015,35(9):32-35.CHENG Yong.Determination of niobium in niobum-iron alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2015,35(9):32-35.
[9]
黎涛,冯自平,陈金发,等.电感耦合等离子体原子发射光谱法测定偏钒酸铵中钒含量[J].理化检验:化学分册,2011,47(9):1086-1087.LI Tao,FENG Zi-ping,CHEN Jin-fa,et al.ICP-AES determination of vanadium in ammonium metavanadate[J].Physical Testing and Chemical Analysis Part B: Chemical Analysis,2011,47(9):1086-1087.
[10]
赵君威,梅坛,鄢国强,等.电感耦合等离子体原子发射光谱分析中的光谱干扰及其校正的研究进展[J].理化检验:化学分册,2013,49(3):334-339.ZHAO Jun-wei,MEI Tan,YAN Guo-qiang.Spectral interference and its correction in ICP-AES analysis[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(3):334-339.
