Abstract:The complex high-salt matrix of nickel electrolyte has interference with the monitoring of micro copper. In this experiment, the rotating disk electrode atomic emission spectrometry was combined with standard addition method. The sample pretreatment was not required and there was no matrix effect. The improved calibration curve was used to determine the micro copper in different intermediate solution of nickel electrolyte. According to the evaporation curve of element, the pre-combustion time of 6 s and acquisition time of 7-30 s were determined. The precombustion excitation improved the wettability of the disk electrode, thus ensuring the stability of the injection quantity. Reasonable exposure time could improve the analysis speed on the premise of ensuring the intensity sensitivity of analytical elements, and the single detection time was less than 35 s. Ni 324.845 7 nm was selected as the internal standard to correct the excitation behavior and injection volume error. The limit of detection was 0.15 mg/L. The content of micro copper in different intermediate solution of nickel electrolyte was determined according to the experimental method. The relative standard deviations (RSD, n=6) were less than 12%, and the recoveries were between 98% and 110%.
[1] 王得祥,卢建波,李亦婧,等.基于硫化镍除铜反应的化学添加剂对电解镍质量影响研究[J].材料导报,2015,29(S1):280-283. WANG Dexiang,LU Jianbo,LI Yijing,et al.The influence of additives on copper removing and electrolytic nickel’s quality[J].Materials Guide,2015,29(S1):280-283. [2] 石玉臣,赵中伟,陈爱良,等.金川镍阳极液硫化除铜的研究[J].有色金属(冶炼部分),2010,61(2):9-12. SHI Yuchen,ZHAO Zhongwei,CHEN Ailiang,et al.Study of removing copper from nickel anode electrolyte by sulfide method[J].Nonferrous Metals(Extractive Metallurgy),2010,61(2):9-12. [3] 方迪,张艳峰.火焰原子吸收光谱法测定锡阳极泥中铜的含量[J].中国无机分析化学,2020,10(5):40-43. FANG Di,ZHANG Yanfeng.Determination of copper elements in tin anode slime by flame atomic absorption spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2020,10(5):40-43. [4] 徐艳燕,朱国忠,柴瑾瑜,等.电感耦合等离子体原子发射光谱法测定钴产品生产过程净化液中12种微量元素[J].冶金分析,2018,38(12):26-35. XU Yanyan,ZHU Guozhong,CHAI Jinyu,et al.Determination of twelve microelements in purified solution during production process of cobalt products by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(12):26-35. [5] 陈磊磊,袁锡泰,余长合,等.电感耦合等离子体质谱(ICP-MS)法测定环境水样中5种重金属元素[J].中国无机分析化学,2017,7(4):11-15. CHEN Leilei,YUAN Xitai,YU Changhe,et al.Determination of five heavy metal elements in ground water by inductively coupled plasma-mass spectrometry(ICP-MS)[J].Chinese Journal of Inorganic Analytical Chemistry,2017,7(4):11-15. [6] 赵新建,吴和平,曹云松,等.标准加入法测定生态水泥中的重金属[J].环境保护科学,2013,39(4):114-119. ZHAO Xinjian,WU Heping,CAO Yunsong,et al.Determination of heavy metal in eco-cement by standard addition method[J].Environmental Protection Science,2013,39(4):114-119. [7] 肖彩林,谭爱民.自动标准加入法测定电解净化液中铜[J].理化检验(化学分册),1997,33(4):172-173. XIAO Cailin,TAN Aimin.Determination of copper in electrolytic purification solution by automatic standard addition method[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),1997,33(4):172-173. [8] 国家国防科技工业局.HB 20094.1—2012航空工作液中磨损金属含量检测 第1部分:转盘电极原子发射光谱仪检测法[S].北京:中国航空综合技术研究所,2013. [9] American Society for Testing Material.D6595-17 Standard test method for determination of wear metal and contamination in used lubricating oils or used hydraulic fluids by rotating disc electrode atomic emission spectrometry[S].United States:ASTM,2017. [10] 吴冬梅,赵燕秋,付国余,等.电弧发射光谱法以两种方式拟合标准曲线分段测量地球化学样品中银[J].冶金分析,2021,41(11):49-56. WU Dongmei,ZHAO Yanqiu,FU Guoyu,et al.Determination of silver in geochemical sample by arc emission spectrometry with segmented curves in two fitting ways[J].Metallurgical Analysis,2021,41(11):49-56. [11] 赵燕秋,吴冬梅,付国余,等.溶液缓冲剂发射光谱法在地质样品多元素测定中的应用[J].分析仪器,2019,9(6):54-61. ZHAO Yanqiu,WU Dongmei,FU Guoyu,et al.Application of solution buffer emission spectrometry in multielement determination of geological samples[J].Analytical Instrumentation,2019,9(6):54-61. [12] 邓勃,周晓慧.火焰原子吸收分光光度法测定镍电解液中微量钴、铜、铁、铅、锌[J].清华大学学报,1980,20(3):79-86. DENG Bo,ZHOU Xiaohui.Determination of trace cobalt,copper,iron,lead and zinc in nickel electrolyte by FAAS[J].Journal of Qinghua University,1980,20(3):79-86. [13] 李文虎,潘勇,雷维新,等.等离子体处理对石墨膜表面亲水性的影响[J].表面技术,2018,47(4):35-41. LI Wenhu,PAN Yong,LEI Weixin,et al.Effect of plasma treatment on surface hydrophilicity of graphite film[J].Surface Technology,2018,47(4):35-41. [14] 李振东,詹华,王亦奇,等.等离子体刻蚀前处理对碳基薄膜结合力的影响[J].表面技术,2017,46(1):64-68. LI Zhendong,ZHAN Hua,WANG Yiqi,et al.Effects of plasma etching pretreatment on adhesion of carbon-based film[J].Surface Technology,2017,46(1):64-68.