Determination of twelve microelements in purified solution duringproduction process of cobalt products by inductively coupledplasma atomic emission spectrometry
XU Yan-yan1,2, ZHU Guo-zhong1,2, CHAI Jin-yu3, HAN Feng3, PAN Li-juan1,2, ZHANG Ke-cui1,2
1. National Nickel and Cobalt Advanced Materials Engineering Research Center, Lanzhou 730101, China; 2. Lanzhou Jinchuan Advanced Materials Technology Co., Ltd., Jinchang 737100, China; 3. Jinchuan Corporation, Ltd., Jinchang 737100, China
Abstract：The cobalt chloride purified solution and cobalt nitrate purified solution during production process of cobalt products contained a lot of cobalt ions. Usually,12 impurity elements in it, including Cu, Fe, Ni, Cd, Zn, Mn, Ca, Mg, Na, Si, As and S, were determined by matrix matching-atomic absorption spectrometry or extraction separation-spectrophotometry. However, these methods had some disadvantages such as long analytical time, complicated operation and high cost. Moreover, only single element could be determined at one time. Thus, inductively coupled plasma atomic emission spectrometry (ICP-AES) was proposed for determination of these elements in purified solution during production process of cobalt products. Under the optimized working conditions of instrument, the influence of matrix effect and instrumental fluctuation could be effectively overcome with internal standard method. The linear correlation coefficients of calibration curves of elements were all higher than 0.999 9. The detection limits of method were between 0.00003g/L and 0.00026g/L. The contents of Cu, Fe, Ni, Cd, Zn, Mn, Ca, Mg, Na, Si, As and S in two systems during production process of cobalt products, i.e., cobalt chloride purified solution and cobalt nitrate purified solution, were determined according to the experimental method. The relative standard deviations (RSD, n=11) of determination results were between 2.8% and 8.9%. The recoveries were between 93% and 107%. The proposed method was applied for determination of Cu, Fe, Ni, Cd, Zn, Mn, Ca, Mg, Na, Si, As and S in cobalt certified reference material for spectral analysis. The results were consistent with the certified values.
苏耀东,覃俐,马红梅.磷酸钕共沉淀火焰原子吸收光谱法测定硫酸钴中痕量铅和铁[J].冶金分析,2004,24(6):36-38.SU Yao-dong,ZHAO Li,MA Hong-mei.Determination of trace lead and iron in cobalt sulfate by flame atomic absorption spectrometry after coprecipitation with neodymium phosphate[J].Metallurgical Analysis,2004,24(6):36-38.
[5]
赵普琇.原子吸收光谱法测定钴粉中镍[J].冶金分析,2012,32(2):51-54.ZHAO Pu-xiu.Determination of nickel in cobalt powder by atomic absorption spectrometry[J].Metallurgical Analysis,2012,32(2):51-54.
[6]
张立岩,王国强,杨润仁.流动注射在线共沉淀火焰原子吸收光谱法测定氯化钴溶液中痕量铅[J].冶金分析,2013,33(5):46-49.ZHANG Li-yan,WANG Guo-qiang,YANG Run-ren.Determination of trace lead in cobalt chloride solution by flow injection on-line coprecipitation flame atomic absorption spectrometry[J].Metallurgical Analysis,2013,33(5):46-49.
[7]
李述信.原子吸收光谱分析中的干扰及消除方法[M].北京:北京地质出版社,1987.
[8]
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.
[9]
王锦荣,董启太.铝合金中锌、铁的快速测定-原子吸收分光光度法[J].山西化工,2004(1):30-34.WANG Jin-rong,DONG Qi-tai.Measurement of Zn and Fe in aluminium alloy-the atomic absorption photometric spectra[J].Shanxi Chemical Industry,2004(1):30-34.
[10]
成勇.电感耦合等离子体原子发射光谱法测定硫酸氧钒中钙镁镍铜铝铁[J].冶金分析,2016,36(2):65-70.CHENG Yong.Determination of calcium,magnesium,nickel,copper,aluminum and iron in vanadyl sulfate by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2016,36(2):65-70.
[11]
任慧萍,王纪华,赵金莲.微量进样原子吸收光谱法测定镍基溶液中微量锌[J].甘肃科技,2013,29(1):44-47.REN Hui-ping,WANG Ji-hua,ZHAO Jin-lian.Determination of trace element of Zn in nickel solutions by microsample introduction-atomic absorption spectrometry[J].Gansu Science Technology,2013,29(1):44-47.
[12]
胡艳君,陈晶玮,曾贤明.电感耦合等离子体原子发射光谱法测定纯铜中杂质元素[J].冶金分析,2009,29(7):40-43.HU Yan-jun,CHEN Jing-wei,ZENG Xian-ming.Determination of impurity elements in pure copper by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2009,29(7):40-43.
[13]
陈希,郭方遒,黄兰芳,等.电感耦合等离子体原子发射光谱法同时测定锌电解液中铜镉钴[J].冶金分析,2012,32(11):51-55.CHEN Xi,GUO Fang-qiu,HUANG Lan-fang,et al.Simultaneous determination of copper,cadmium and cobalt in zinc electrolyte by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2012,32(11):51-55.
[14]
张斯美,吴银军,段宏然.用ICP-AES法同时测定锰矿中氧化钙、氧化镁、钴、镍、锌、铅、铜含量的应用[J].铁合金,2011(6):39-43.ZHANG Si-mei,WU Yin-jun,DUAN Hong-ran.Simultaneous determination of CaO,MgO,Co,Ni,Zn,Pb and Cu content in manganess ore by ICP-AES method[J].Ferro Alloys,2011(6):39-43.
[15]
李建,计辉,钱玉萍.电感耦合等离子体发射光谱法(ICP-OES)同时测定活性炭中铝、钴、镉、铜、铁、镁、锰、钠、磷、硫10种元素[J].中国无机分析化学,2012,2(1):58-60.LI Jian,JI Hui,QIAN Yu-ping.Simultaneous determination of Al,Co,Cr,Cu,Fe,Mg,Mn,Na,P and S in activated carbon by inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2012,2(1):58-60.
[16]
菅豫梅,王培.ICP-AES法快速测定金属钴粉中的九种杂质元素[J].湖南有色金属,2009,25(6):57-61.JIAN Yu-mei,WANG Pei.Nine impurity elements′determination in the metallic cobalt powders by ICP-AES method[J].Hunan Nonferrous Metals,2009,25(6):57-61.
[17]
王凌,冉文生,张辽生,等.电感耦合等离子体原子发射光谱法测定电解钴中杂质元素[J].福建分析测试,2011,20(6):27-29.WANG Ling,REN Wen-sheng,ZHANG Liao-sheng,et al.Inductively coupled plasma atomic emission spectrometry determination of impurity elements in electrolytic cobalt[J].Fujian Analysis & Testing,2011,20(6):27-29.
[18]
龚琦.对电感耦合等离子体发射光谱法中一些问题的认识[J].冶金分析,2018,38(9):26-30.GONG Qi.Understanding of some issues about inductively coupled plasma optical emission spectrometry[J].Metallurgical Analysis,2018,38(9):26-30.
