电感耦合等离子体原子发射光谱法测定钨镧合金中镧  

Determination of lanthanum in tungsten-lanthanum alloy by inductively coupled plasma atomic emission spectrometry

作　　者：杨相庚 盛力 袁冬梅 卢博 YANG Xianggeng;SHENG Li;YUAN Dongmei;LU Bo(National Center of Quality Testing and Inspection for Tungsten and Rare Earth Products,Ganzhou 341000,China;Jiangxi Institute of Tungsten and Rare Earth,Ganzhou 341000,China)

机构地区：[1]国家钨与稀土产品质量检验检测中心,江西赣州341000 [2]江西省钨与稀土研究院,江西赣州341000

出　　处：《冶金分析》2025年第1期91-95,共5页Metallurgical Analysis

摘　　要：采用三氧化二镧对钨合金进行细晶强化与弥散强化一直是研究的热门,镧含量直接影响着钨镧合金的性能,因此对钨镧合金制品中镧含量的准确分析很有必要。实验使用硝酸和氢氟酸溶解样品,然后加入柠檬酸和磷酸-高氯酸混合酸用于络合溶解出的钨及驱赶氢氟酸,再次加入过氧化氢、柠檬酸、硝酸溶解盐类,解决了钨镧合金消解效率慢及消解过程中易产生钨酸沉淀的问题;选用La 379.082 nm作为镧的分析谱线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定钨镧合金中镧的方法。结果表明:镧的质量浓度在2.00~50.0μg/mL范围内与其发射强度呈线性关系,线性相关系数大于0.999 9;方法中镧的检出限为0.000 25%,镧的定量限为0.001 2%;钨镧合金中钨、磷、锆、钍等共存元素对镧的测定无干扰。按照实验方法测定钨镧合金中镧,结果的相对标准偏差(RSD,n=6)为0.89%~1.2%,加标回收率为97%~100%。The use of lanthanum trioxide for fine crystal strengthening and dispersion strengthening of tungsten alloy has always been a hot research topic.The content of lanthanum directly affects the properties of tungsten-lanthanum alloy,so it is necessary to accurately analyze the content of lanthanum in tungsten-lanthanum alloy products.In this study,the sample was dissolved with nitric acid and hydrofluoric acid.Then citric acid and phosphoric acid-perchloric acid was added for the complexation of dissolved tungsten and remove hydrofluoric acid.Hydrogen peroxide,citric acid and nitric acid were then added to dissolve the salts.The pretreatment method solved the problems of slow digestion efficiency and easy formation of tungstic acid precipitation during the digestion process of tungsten-lanthanum alloy.La 379.082 nm was selected as the analytical line.A method for the determination of lanthanum in tungsten-lanthanum alloy by inductively coupled plasma atomic emission spectrometry(ICP-AES) was established.The results showed that the mass concentration of lanthanum in range of 2.00-50.0 μg/mL had a linear relationship to the corresponding emission intensity,and the linear correlation coefficient was greater than 0.999 9.The limit of detection and limit of quantification of lanthanum were 0.000 25% and 0.001 2%,respectively.The coexisting elements in tungsten-lanthanum alloys such as tungsten,phosphorus,zirconium,and thorium had no interference with the determination of lanthanum.The content of lanthanum in tungsten-lanthanum alloy was determined according to the experimental method.The relative standard deviations(RSD, n=6) of determination results were between 0.89% and 1.2%,and the recoveries were between 97% and 100%.

关 键 词：钨镧合金 镧 电感耦合等离子体原子发射光谱法(ICP-AES) 

分 类 号：O657.31[理学—分析化学]