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  

Determination of total content of zirconium oxide and hafnium oxide in cerium-zirconium composite oxide by mandelic acid gravimetry

作　　者：王丽娟 赵拓 李蒙 任旭东 张慧珍[1,2] WANG Lijuan;ZHAO Tuo;LI Meng;REN Xudong;ZHANG Huizhen(State Key Laboratory for Research and Comprehensive Utilization of Rare Earth Resources in Bayan Obo,Baotou 014030,China;Baotou Research Institute of Rare Earths,Baotou 014030,China;Inner Mongolia Rare Earth Ovonic Metal Hydride Co.,Ltd.,Baotou 014030,China)

机构地区：[1]白云鄂博稀土资源研究与综合利用国家重点实验室,内蒙古包头014030 [2]包头稀土研究院,内蒙古包头014030 [3]内蒙古稀奥科贮氢合金有限公司,内蒙古包头014030

出　　处：《冶金分析》2023年第8期69-73,共5页Metallurgical Analysis

摘　　要：氧化锆和氧化铪合量为铈锆复合氧化物性能的重要评价指标。采用10 mL硝酸、1滴氢氟酸加热溶解试样至试液清亮,加入5.0 mL硫酸(1+1),在电炉上加热至冒尽白烟,取下冷却,用10 mL盐酸和2.0 mL过氧化氢进行提取,用氨水分离法除去钙、镁和硫酸根后,加入苦杏仁酸溶液沉淀锆和铪,生成难溶性的苦杏仁酸锆铪白色絮状沉淀,陈化后于900℃灼烧,以氧化物形式称重,经过计算得出试样中氧化锆和氧化铪的合量。据此,建立了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的方法。采用实验方法测定铈锆复合氧化物样品中氧化锆和氧化铪合量,测定结果的相对标准偏差(RSD,n=11)为0.46%和0.23%。用不含氧化锆和氧化铪的高纯氧化铈、高纯氧化镧、高纯氧化镨和基准试剂氧化锆配制铈锆复合氧化物模拟试样,按照实验方法对氧化锆和氧化铪合量进行测定,结果表明,测定值与理论值基本一致。采用实验方法、X射线荧光光谱法和电感耦合等离子体原子发射光谱法对铈锆复合氧化物控制样中氧化锆和氧化铪合量进行测定。结果表明,3种方法的测定值均与参考值基本一致。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 r

关 键 词：铈锆复合氧化物 苦杏仁酸 重量法 氧化锆 氧化铪 合量 

分 类 号：O655.24[理学—分析化学] TF845[理学—化学]