Application of electrolytic gravimetry and inductively coupled plasma atomic emission spectrometry in the determination of nickel, cobalt, copper, zinc, iron and manganese in nickel oxide
HU Jian-chun, ZHAO Jin,ZHANG Rui-lin
Technology Center, Shanxi Taigang Stainless Steel Co., Ltd., Taiyuan 030003, China
Abstract：The nickel oxide sample was dissolved with nitric acid and perchloric acid. After filtration, the nickel in filtrate was determined by constant current electrolytic gravimetry. 10 mL of 500 g/L ammonium citrate solution was added. The pH of electrolyte was 10. The electrolysis current and time was 2 A and 2 h, respectively. Ni 341.486 nm, Co 238.892 nm, Cu 324.752 nm, Zn 206.191 nm, Fe 259.940 nm and Mn 257.610 nm were selected as the analytical lines. The calibration solution was prepared by matrix matching method to eliminate the matrix effect. The cobalt, copper, zinc, iron and manganese deposited on platinum cathode were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Then, the nickel, manganese and iron in electrolytic residual solution and acid-insoluble residue were determined. The content of nickel, manganese and iron was the sum of results obtained from platinum cathode, electrolytic residual solution and acid-insoluble residue. The detection limits of elements in this method were in range of 0.002 4 and 0.020 μg/mL. The linear correlation coefficients of calibration curves were higher than 0.999. The content of nickel, cobalt, copper, zinc, iron and manganese in nickel oxide sample was determined according to the experimental method, and the relative standard deviations (RSD, n=10) of determination results were between 0.11% and 7.5%. The proposed method was applied to the determination of nickel oxide samples, and the found results were consistent with those obtained by the national standard method and atomic absorption spectrometry
胡建春,赵 琎,张瑞霖. 电解重量法和电感耦合等离子体原子发射光谱法在测定氧化镍中镍钴铜锌铁锰中的应用[J]. 冶金分析, 2015, 35(11): 28-33.
HU Jian-chun, ZHAO Jin,ZHANG Rui-lin. Application of electrolytic gravimetry and inductively coupled plasma atomic emission spectrometry in the determination of nickel, cobalt, copper, zinc, iron and manganese in nickel oxide. , 2015, 35(11): 28-33.
王永利.过硫酸铵-丁二酮肟示差分光光度法测定镍铁中的镍 [J]. 东北林业大学学报,2001,29(4):82-83. WANG Yong-li.Ammonium persulfate-dimethylglyoxime differential spectrophotometric method for the determination of nickel in ferronickel [J].Journal of North East Forest University,2001,29(4):82-83.
[3]
顾鸿语,王道尧.用电导法测定镍合金中镍 [J].材料保护,1997(11):40-42. GU Hong-yu,WANG Dao-yao. By electrical conductivity method for the determination of nickel in nickel alloy [J]. Materials Protection,1997(11):40-42.
[4]
刘柏雄,钟素文.电沉积法制备泡沫镍的研究 [J].有色金属科学与工程, 2011,2(3):28-31. LIU Bai-xiong,ZHONG Su-wen.Nickel foam production by electro-deposition [J]. Nonferrous Metals Science and Engineering,2011,2(3):28-31.
[5]
杨丽荣,于媛君,亢德华,等. 电感耦合等离子体原子发射光谱法测定钢中铌钨锆 [J].冶金分析,2014,34(11):51-55. YANG Li-rong,YU Yuan-jun,KANG De-hua,et al.Determination of niobium,tungsten and zirconium in steel by inductively coupled plasma topic emission spectyometry [J].Metallurgical Analysis,2014,34(11):51-55.
[6]
谢华林,刘宏伟.ICP-AES法测定高纯阴极铜中杂质元素 [J].冶金分析,2004,24(3):40-42. XIE Hua-lin,LIU Hong-wei.Determination of impurity elements in high purity copper cathode by ICP-AES[J].Metallurgical Analysis,2004,24(3):40-42.
[7]
刘清平,田荣华. ICP-AES法测定镍粉中铁、钴、铜、锌等 l5个杂质元素 [J].环境与开发,1998,13(4):48-49. LIU Qing-ping,TIAN Rong-hua.Determination of Fe,Co,Cu,Zn ete.15 impurities in nickel powder with ICP-AES [J]. Environment and Development,1998,13(4):48-49.
[8]
邹智敏,郭宏杰,马洪波,等. 电感耦合等离子体原子发射光谱法测定高铬镍基合金中微量钴 [J].冶金分析,2014,34(7):74-77. ZOU Zhi-min,GUO Hong-jie,MA Hong-bo,et al.A method for the determination of trace cobalt in alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(7):74-77.
[9]
戴学谦,胡建春,王君. 电解重量法测定烧结镍中镍 [J].冶金分析,2008,28(8):27-31. DAI Xue-qian,HU Jian-chun,WANG Jun.Determination of nickel in nickel sinter by electrolytic gravimetry [J].Metallurgical Analysis, 2008,28(8):27-31.
[10]
孙宝莲,李波,江燕妮,等.电沉积重量法测定核级-银铟镉合金中银 [J].稀有金属快报,2005,24(11):31-34.SUN Bao-lian,LI Bo,JIANG Yan-ni,et al.Determination of agin nuclear grade Ag-In-Cd alloys by the electrolytic deposition analysis [J].Joural of Rare Metals,2005,24(11): 31-34.
[11]
王金砖,张玉洁,伏荣进,等. 校准曲线和观测方式对电感耦合等离子体原子发射光谱法测定不锈钢中镍、铬和锰的影响 [J]. 冶金分析, 2015,35(1):45-49.WANG Jin-zhuan,ZHANG Yu-jie,FU Rong-jin, et al. Effect of calibration curve and observation way on the determination of nickel,chromium and manganese in stainless steel by inductively coupled plasma atomic emission spectrometry [J]. Metallurgical Analysis, 2015,35(1):45-49.
