电感耦合等离子体原子发射光谱法测定锆英砂中钡  

Determination of barium in zircon sand by inductively coupled plasma atomic emission spectrometry

作　　者：古娟 徐娜 李建国 蒋小岗 GU Juan;XU Na;LI Jianguo;JIANG Xiaogang(National Tungsten&Rare-earth Product Quality Supervision Testing Center,Ganzhou 341000,China)

机构地区：[1]国家钨与稀土产品质量监督检验中心,江西赣州341000

出　　处：《冶金分析》2021年第5期63-68,共6页Metallurgical Analysis

基　　金：有色金属行业标准项目(2018-2038T-YS)。

摘　　要：锆合金和锆化合物广泛应用于航空航天、核能、特种陶瓷玻璃等战略新兴产业,锆英砂作为其重要原料,目前的测试方法不能满足其中钡量的测试需求。实验称取0.5000g样品于覆盖2.0g无水过氧化钠和2.0g无水碳酸钠的银坩埚中,在700℃熔融制样;水浸过滤后以硝酸、高氯酸溶解滤渣,选择Ba 233.527nm作为分析线,建立了使用电感耦合等离子体原子发射光谱法(ICP-AES)测定锆英砂中钡含量的方法。结果表明,钡的质量浓度在0.1~15.0μg/mL范围内与其发射强度呈线性关系,线性相关系数大于0.9999;方法检出限为0.0003%(质量分数,下同),定量限为0.0010%。溶液中共存的300μg/mL硅、50μg/mL铝、50μg/mL铁、10μg/mL铪、100μg/mL钙、200μg/mL锆对1mg/L钡的测定均无影响。按照实验方法测定锆英砂中钡,结果的相对标准偏差(RSD,n=7)小于5%;回收率为98%~102%,测定结果与电感耦合等离子体质谱法的测定结果相吻合。Zirconium alloys and zirconium compounds are widely used in aerospace,nuclear energy,special ceramic glass and other strategic emerging industries.Zirconium sand is an important raw material for zirconium alloys and zirconium compounds,and the current determination methods of barium content cannot meet the testing demand.0.5000 g of sample was transferred into silver crucible containing 2.0 g of anhydrous sodium peroxide and 2.0 g of anhydrous sodium carbonate in experiments followed by fusion sample preparation at 700℃.The filter residue was dissolved with nitric acid and perchloric acid after water leaching and filtering.Ba 233.527 nm was selected as the analytical line to establish the determination method of barium in zircon sand by inductively coupled plasma atomic emission spectrometry(ICP-AES).The results showed that the mass concentration of barium in the range of 0.1-15.0μg/mL was linear to the emission intensity,and the correlation coefficient was greater than 0.9999.The limit of detection(mass fraction,similarly hereinafter)and limit of quantification were 0.0003%and 0.0010%,respectively.The determination of barium was not affected by the following coexisting ions in solution:300μg/mL Si,50μg/mL Al,50μg/mL Fe,10μg/mL Hf,100μg/mL Ca,and 200μg/mL Zr.The content of barium in zircon sand was determined according to the experimental method.The relative standard deviation(RSD,n=7)was less than 5%,and the recoveries were between 98%and 102%.The measurement results were consistent with those obtained by inductively coupled plasma mass spectrometry.

关 键 词：电感耦合等离子体原子发射光谱法(ICP-AES) 锆英砂 钡 

分 类 号：TF802.1[冶金工程—有色金属冶金] O657.31[理学—分析化学]