Determination of total content of zirconium oxide and hafnium oxide in cerium-zirconium composite oxide by mandelic acid gravimetry
WANG Lijuan1,2, ZHAO Tuo1,2, LI Meng3, REN Xudong1,2, ZHANG Huizhen*1,2
1. State Key Laboratory for Research and Comprehensive Utilization of Rare Earth Resources in Bayan Obo, Baotou 014030,China; 2. Baotou Research Institute of Rare Earths,Baotou 014030,China; 3. Inner Mongolia Rare Earth Ovonic Metal Hydride Co.,Ltd.,Baotou 014030,China
Abstract：Total content of zirconium oxide and hafnium oxide is an important evaluation index for the cerium-zirconium composite oxide. The sample was dissolved with 10 mL of nitric acid and one drop of hydrofluoric acid by heating until the solution was clear. Then 5.0 mL of sulfuric acid (1+1) was added and the solution was heated on electric furnace until white smoke disappeared. After cooling, 10 mL of hydrochloric acid and 2.0 mL of hydrogen peroxide were added for extraction. Calcium, magnesium and sulfate were removed by ammonia separation method. Then mandelic acid solution was added to react with zirconium and hafnium to form insoluble white flocculation precipitates. After ageing, the precipitates were calcinated at 900 ℃ and weighed in the form of oxides. Consequently, the total content of zirconium oxide and hafnium oxide in sample could be calculated. Based on this, a method for the determination of total content of zirconium oxide and hafnium oxide in cerium-zirconium composite oxide by mandelic acid gravimetry was established. Total content of zirconium oxide and hafnium oxide in cerium-zirconium composite oxide was determined according to the experimental method. The relative standard deviation (RSD, n=11) of determination results was 0.46% and 0.23%, respectively. The simulated sample of cerium-zirconium composite oxide was prepared using high-purity cerium oxide, high-purity lanthanum oxide, high-purity praseodymium oxide (without zirconium oxide and hafnium oxide) and reference reagent zirconium oxide. The total content of zirconium oxide and hafnium oxide was determined according to the experimental method. The results showed that the found results were basically consistent with the theoretical values. The total content of zirconium oxide and hafnium oxide in control sample of cerium-zirconium composite oxide was determined by the proposed method, X-ray fluorescence spectrometry and inductively coupled plasma atomic emission spectrometry. The results showed that the measured values of three methods were basically consistent with the reference values.
王丽娟, 赵拓, 李蒙, 任旭东, 张慧珍. 苦杏仁酸重量法测定铈锆复合氧化物中氧化锆和氧化铪合量[J]. 冶金分析, 2023, 43(8): 69-73.
WANG Lijuan, ZHAO Tuo, LI Meng, REN Xudong, ZHANG Huizhen. Determination of total content of zirconium oxide and hafnium oxide in cerium-zirconium composite oxide by mandelic acid gravimetry. , 2023, 43(8): 69-73.
[1] 龙志奇,崔梅生,朱兆武,等.铈锆复合氧化物的研究、应用与展望[J].稀有金属快报,2007(1):40-44. LONG Zhiqi,CUI Meisheng,ZHU Zhaowu,et al.Progress for application and preparation of ceria-zirconia composite and prospects for the markets[J].Rare Metals Letters,2007(1):40-44. [2] 彭新林,龙志奇,崔梅生,等.共沉淀法合成铈锆复合氧化物及表征[J].中国稀土学报,2002(S2):104-107. PENG Xinlin,LONG Zhiqi,CUI Meisheng,et al.Coprecipitation synthesis cerium zirconium composite oxide and characterization[J].Journal of China's Rare Earths,2002(S2):104-107. [3] 张宏,白英芝,王海彦.含锆复合氧化物催化剂的制备方法研究进展[J].辽宁石油化工大学学报,2019,39(1):35-38. ZHANG Hong,BAI Yingzhi,WANG Haiyan.The preparation method of zirconium compound oxide catalyst research progress[J].Journal of Liaoning University of Petroleum and Chemical,2019,33(1):35-38. [4] 国家发展和改革委员会.YS/T568.1—2008 氧化锆、氧化铪化学分析方法 氧化锆和氧化铪合量的测定 苦杏仁酸重量法[S].北京:中国标准出版社,2008. [5] 王素梅,张慧珍,李净岩,等.氧化钇稳定氧化锆中氧化锆含量的测定[J].稀土,2015(3):105-108. WANG Sumei,ZHANG Huizhen,LI Jingyan,et al.Determination of zirconium oxide content in yttria stabilized zirconia[J].Chinese Rare Earths,2015(3):105-108. [6] 张嘉祺,冯典英,巩琛,等.电感耦合等离子体原子发射光谱法测定铪合金中锆[J].化学分析计量,2022(10):54-57. ZHANG Jiaqi,FENG Dianying,GONG Chen,et al.Determination of zirconium in hafnium alloy by inductively coupled plasma optical emission spectrometry[J].Chemical Analysis and Meterage,2022(10):54-57. [7] 颜晓华,魏修宇,石建光.电感耦合等离子体原子发射光谱法测定钼基合金中钛、钽、锆量[J].硬质合金,2021,38(6):441-445. YAN Xiaohua,WEI Xiuyu,SHI Jianguang.Determination of titanium,tantalum and zirconium in molybdenum base alloy by inductively coupled plasma atomic emission spectrometry[J].Cemented Carbide,2021,38(6):441-445. [8] 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 Lirong,YU Yuanjun,KANG Dehua,et al.Determination of niobium,tungsten and zirconium in steel by inductively coupled plasma atomic emission spectrometry[J].Metallurgicall Analysis,2014,34(11):51-55. [9] 王杰平,刘美芳,于龙飞,等.快速高压消解-电感耦合等离子体质谱法同时测定地质样品中的锆、铪[J].吉林地质,2022(1):79-83. WANG Jieping,LIU Meifang,YU Longfei,et al.Simultaneous determination of zirconium and hafnium in geological samples by rapid high pressure digestion inductively coupled plasma mass spectrometry[J].Jilin Geology,2022(1):79-83. [10] 王志彪,关海兰.熔融制样-X射线荧光光谱法测定锆质耐火材料中11种主次组分[J].冶金分析,2022,42(3):78-83. WANG Zhibiao,GUAN Hailan.Determination of eleven major and minor components in zirconize refractory by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgicall Analysis,2022,42(3):78-83. [11] 卢才兴,李志文,王彬,等.熔融制样-X射线荧光光谱法测定铈锆固溶体中的元素成分[J].工业催化,2019(9):78-82. LU Caixing,LI Zhiwen,WANG Bin,et al.Determination of elemental components in cerium-zirconium solid solution by melt sample preparation X-ray fluorescence spectrometry[J].Industrial Catalysis,2019(9):78-82. [12] 周双清,徐建平,李明昌.粉末压片制样-X射线荧光光谱法测定二氧化锆材料中二氧化锆的含量[J].理化检验(化学分册),2022,58(8):902-908. ZHOU Shuangqing,XU Jianping,LI Mingchang.Determination of zirconium dioxide in zirconium dioxide material by X-ray fluorescence spectrometry after sample preparation with powder tableting[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2022,58(8):902-908. [13] 董雪平,周新木,陈慧勤,等.P507萃取分离-二甲酚橙光度法测定锆铪[J].分析科学学报,2009,25(5):563. DONG Xueping,ZHOU Xinmu,CHEN Huiqin,et al.Extraction separation and spectrophotometric determination of zirconium and hafnium[J].Journal of Analytical Science,2009,25(5):563. [14] 中华人民共和国工业和信息化部.XB/T 518—2021铈锆复合氧化物[S].北京:冶金工业出版社,2021.
