Discussion on determination method of nickel in high-cobalt-nickel material by EDTA titration with ammonium persulfate masking cobalt and dimethylglyoxime precipitation separation
ZUO Hua
Hunan Research Institute for Nonferrous Metals Co.,Ltd.,Changsha 410100,China
Abstract：Accurate determination of nickel content in high-cobalt-nickel material is of great significance for the purification technology study and industry development of nickel smelting. The mass fraction of cobalt in high-cobalt-nickel material is usually in range of 10%-20% or even higher. When nickel in this sample is determined by EDTA titration with dimethylglyoxime precipitation separation, cobalt will have interference. In this paper, ammonium persulfate was added to oxidize cobalt (Ⅱ) to cobalt (Ⅲ), which would exist in solution in the form of [Co(NH3)6]3+. Thus, the interference of cobalt (Ⅱ) with the precipitation reaction between dimethylglyoxime and nickel would be avoided. Then the content of nickel in precipitate was determined by EDTA titration with dimethylglyoxime precipitation separation. Meanwhile, the content of nickel in filtrate was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) to correct the results of titration. Therefore, the determination of nickel in high-cobalt-nickel material was realized. The influence of cobalt content on the determination of nickel was investigated. The possibility of increasing dimethylglyoxime ethanol solution dosage to eliminate this interference was also studied. The results showed that cobalt in the sample had interference with nickel determination, and the interference could not be eliminated by increasing dimethylglyoxime dosage. The oxidization conditions of cobalt (Ⅱ) by ammonium persulfate were optimized. The results showed that cobalt (Ⅱ) could be completely oxidized and the excessive ammonium persulfate could be fully decomposed under such conditions: the pH of solution was adjusted to 6-10 with ammonium hydroxide(1+1); after adding 10 mL of 50 g/L ammonium persulfate solution, the solution was boiled with soft fire for 10 min. The contents of nickel in 2 samples of high-cobalt-nickel material were determined according to the proposed method. Moreover, the standard addition tests were conducted. The relative standard deviations (RSD, n=7) of determination results were between 0.14% and 0.59%, and the recoveries were between 99.8% and 100.8%. The contents of nickel in 2 samples of high-cobalt-nickel material were determined according to the proposed method and standard method of GB/T 30072-2013. The statistical analysis of the results by two methods was conducted by t test. The results showed that t<t7,0.05=2.18, indicating that there was no significant difference between the two above methods.
左花. 过硫酸铵掩蔽钴-丁二酮肟沉淀分离-EDTA滴定法测定高钴镍物料中镍方法的探讨[J]. 冶金分析, 2024, 44(9): 83-90.
ZUO Hua. Discussion on determination method of nickel in high-cobalt-nickel material by EDTA titration with ammonium persulfate masking cobalt and dimethylglyoxime precipitation separation. , 2024, 44(9): 83-90.
[1] 国家发展和改革委员会.YS/T 341.1—2006镍精矿化学分析方法 镍量的测定 丁二酮肟沉淀分离EDTA滴定法[S].北京:中国标准出版社,2006. [2] 付海阔,何海梅.丁二酮肟沉淀分离-EDTA滴定法测定镍钴锰三元氢氧化物中镍[J].冶金分析,2020,40(7):47-51. FU Haikuo,HE Haimei.Determination of nick-cobalt-manganese composite hydroxide by EDTA titration after precipitation separation using dimethylglyoxime[J].Metallurgical Analysis,2020,40(7):47-51. [3] 陆娜萍,年季强,张良芬,等.EDTA滴定法测定镍镁合金中镍和镁[J].冶金分析,2016,36(1):62-66. LU Naping,NIAN Jiqiang,ZHANG Liangfen,et al.Determination of nickel and magnesium in nickel-magnesium alloy by EDTA titrimetry[J].Metallurgical Analysis,2016,36(1):62-66. [4] 祁玉静,范丽新.Na2EDTA返滴定法测定铜镍合金中的镍含量[J].中国无机分析化学,2021,11(2):62-65. QI Yujing,FAN Lixin.Determination of nickel in crude copper by Na2EDTA back titration[J].Chinese Journal of Inorganic Analytical Chemistry,2021,11(2):62-65. [5] 朱贤学,沈玉力,康开斌,等.微波消解-丁二酮肟沉淀分离-EDTA返滴定法测定含镍生铁中镍[J].冶金分析,2021,41(11):71-77. ZHU Xianxue,SHEN Yuli,KANG Kaibin,et al.Determination of nickel in nickel pig iron by microwave digestion dimethylglyoxime precipitation separation-EDTA back titration[J].Metallurgical Analysis,2021,41(11):71-77. [6] 许洁瑜,麦丽碧,陈晓东.丁二酮肟分离-EDTA络合返滴定法测定哈氏合金中的镍[J].材料研究与应用,2015,9(1):65-68. XU Jieyu,MAI Libi,CHEN Xiaodong.Determination of nickel in hastelloy alloy by dimethylglyoxime separation-EDTA complex back titration[J].Materials Research and Application,2015,9(1):65-68. [7] 国家发展和改革委员会.YS/T 252.1—2007 高镍锍化学分析方法 镍量的测定 丁二酮肟重量法[S].北京:中国标准出版社,2007. [8] 陈兰,胡军凯,潘晓玲,等.硫代硫酸钠掩蔽铜-丁二酮肟重量法测定含铜工业硫酸镍中镍[J].冶金分析,2018,38(6):66-69. CHEN Lan,HU Junkai,PAN Xiaoling,et al.Determination of nickel in copper-containing industrial nickel sulfate by dimethylglyoxime gravimetry after masking copper with sodium thiosulfate[J].Metallurgical Analysis,2018,38(6):66-69. [9] 谢英豪,明帮来,余海军,等.丁二酮肟重量法测定镍钴铝氢氧化物中镍含量[J].广州化工,2021,49(1):60-62. XIE Yinghao,MING Banglai,YU Haijun,et al.Determination of nickel content in nickel cobalt aluminum hydroxide by dimethylglyoxime gravimetric method[J].Guangzhou Chemical Industry,2021,49(1):60-62. [10] 付海阔.酒石酸掩蔽铝-丁二酮肟重量法测定镍钴铝三元氢氧化物中镍[J].中国无机分析化学,2020,10(6):37-40. FU Haikuo.Determination of nickel in nickel cobalt aluminium composite hydroxide by dimethylglyoxime gravimetry following masking aluminium with tartaric acid[J].Chinese Journal of Inorganic Analytical Chemistry,2020,10(6):37-40. [11] 冯朝军,曾静.丁二酮肟重量法测定冶炼副产品硫酸镍中镍含量[J].资源环境与工程,2019,33(4):593-596. FENG Zhaojun,ZENG Jing.Determination of nickel content in nickel sulfate by dimethylglyoxime gravimetry[J].Resources Environment ＆ Engineering,2019,33(4):593-596. [12] 许洁瑜,王芳,张永进.微波消解-丁二酮肟分光光度法测定钴铬钨系合金粉末中镍[J].冶金分析,2022,42(6):80-84. XU Jieyu,WANG Fang,ZHANG Yongjin.Determination of nickel in cobalt-chromium-tungsten alloy powd-er by dimethylglyoxime spectrophotometry with microwave digestion[J].Metallurgical Analysis,2022,42(6):80-84. [13] 王彤,冯振华,徐进勇,等.分光光度法测定高铁﹑高镁红土镍矿中的镍[J].中国无机分析化学,2012,2(2):20-23. WANG Tong,FENG Zhenhua,XU Jinyong,et al.Determination of nickel in latrite-nickel ore with high iron and high magnesium by spectrophotometry[J].Chinese Journal of Inorganic Analytical Chemistry,2012,2(2):20-23. [14] 赖雪芳.高镍合金中镍含量方法研发[J].广东化工,2023,50(20):15-18. LAI Xuefang.Research and development of nickel content methods in high nickel alloys[J].Guangdong Chemical Industry,2023,50(20):15-18. [15] 褚宁,蒋晓光,李卫刚,等.过硫酸铵-丁二酮肟光度法测定红土镍矿中的镍[J].岩矿测试,2012,31(3):479-483. CHU Ning,JIANG Xiaoguang,LI Weigang,et al.Determination of nickel in nickel laterite ores by ammonium persulfate-dimetylglyoxime spectrophotometry[J].Rock and Mineral Analysis,2012,31(3):479-483. [16] 徐盘明,赵祥大.实用金属材料分析方法[M].北京:中国科技大学出版社,1990:572. [17] 刘绍璞.金属化学分析概论与应用[M].成都:四川科技出版社,1985:218. [18] 马丽君,邵纯红.重量法测定金属镍的改进[J].化学工程师,2002(2):66-67. MA Lijun,SHAO Chunhong.Improvement of gravimetric method for measurement of nickel in alloy[J].Chemical Engineer,2002(2):66-67. [19] 中华人民共和国工业和信息化部.YS/T 928.3—2013镍、钴、锰三元素氢氧化物化学分析方法 第3部分:镍、钴、锰量的测定 电感耦合等离子体发射光谱法[S].北京:中国标准出版社,2013. [20] 北京矿冶研究院总院.矿石及有色金属分析手册[M].北京:冶金工业出版社,1990:68-69. [21] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 30072—2013 镍铁 镍含量的测定 EDTA滴定法[S].北京:中国标准出版社,2013. [22] 中华人民共和国工业和信息化部.YS/T 341.5—2020 镍精矿化学分析方法 第5部分:铜、铅、锌、镁、镉和砷含量的测定 电感耦合等离子体原子发射光谱法[S].北京:中国标准出版社,2020.
