碱熔-电感耦合等离子体原子发射光谱法测定钨精矿中钡  

Determination of barium in tungsten concentrate by inductively coupled plasma atomic emission spectrometry with alkali fusion

作　　者：李平 徐娜 肖石妹 李建国 LI Ping;XU Na;XIAO Shimei;LI Jianguo(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》2024年第3期46-52,共7页Metallurgical Analysis

基　　金：有色金属行业标准项目(20202880-T-610)。

摘　　要：钨精矿作为钨产品的重要原料,其中的钡会与钨形成难溶的沉淀,故钡含量直接影响钨产品的品质及回收率。实验称取0.5000 g样品于盛有2 g无水碳酸钠的银坩埚中,覆盖1 g氢氧化钠、1 g过氧化钠和0.1 g氯化锶,在700℃熔融15 min;水浸过滤后以硝酸、高氯酸溶解滤渣;选择Ba 455.40 nm作为分析线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定钨精矿中钡的方法。结果表明:钡的质量浓度在0.5~10.0μg/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。钨精矿中铁、钙、镁、锰、镍等共存元素对钡的测定无干扰;方法检出限为0.00078%,定量限为0.0026%。按照实验方法测定钨精矿样品中钡,结果的相对标准偏差(RSD,n=11)为1.4%~1.6%,回收率为92%~105%。8个实验室采用实验方法对钨精矿样品中钡进行测定,统计数据结果表明该方法精密度满足产品检测需求,并形成国家标准方法进行推广。Tungsten concentrate is an important raw material of tungsten products.Barium in tungsten concentrate could form insoluble precipitate with tungsten,so the content of barium will directly affect the quality and yield of tungsten products.0.5000 g of sample was weighed and transferred into a silver crucible containing 2 g of anhydrous sodium carbonate,then covered with 1 g of sodium hydroxide,1 g of sodium peroxide and 0.1 g of strontium chloride.The mixture was melted at 700℃for 15 min.After water leaching and filtration,the residue was dissolved with nitric acid and perchloric acid.Consequently,a method for determination of barium in tungsten concentrate was established by inductively coupled plasma atomic emission spectrometry(ICP-AES)with Ba 455.40 nm as analytical line.The results showed that the mass concentration of barium in range of 0.5-10.0μg/mL had a linear relationship with its corresponding emission intensity,and the linear correlation coefficient was greater than 0.9999.The coexisting elements such as iron,calcium,magnesium,manganese and nickel in tungsten concentrate did not interfere with the determination of barium.The limit of detection and the limit of quantification was 0.00078%and 0.0026%,respectively.The contents of barium in tungsten concentrate samples were determined according to the proposed method.The relative standard deviations(RSD,n=11)of determination results were between 1.4%and 1.6%,and the recoveries were between 92%and 105%.The proposed method was used in 8 laboratories for determination of barium in tungsten concentrate samples.The results of statistical data analysis showed that its precision could meet the requirements of product testing,and a national standard method was formed for promotion.

关 键 词：钨精矿 钡 碱熔 电感耦合等离子体原子发射光谱法(ICP-AES) 银坩埚 

分 类 号：O657.31[理学—分析化学] TF031[理学—化学] TF841.1[冶金工程—冶金物理化学]