电感耦合等离子体原子发射光谱法测定Si-B-C-N陶瓷材料中的硅和硼  

Determination of silicon and boron in Si-B-C-N ceramics by inductively coupled plasma atom emission spectrometry

作　　者：刘悦婷 刘亮[1] 徐林[1] 卢鹉[1] LIU Yueting;LIU Liang;XU Lin;LU Wu(Aerospace Research Institute of Materials&Processing Technology,Beijing 100076,China)

机构地区：[1]航天材料及工艺研究所,北京100076

出　　处：《化学分析计量》2023年第7期7-11,共5页Chemical Analysis And Meterage

摘　　要：建立了电感耦合等离子体原子发射光谱法同时测定Si-B-C-N陶瓷材料中硅和硼元素含量的方法。将SiB-C-N陶瓷材料粉碎过孔径为75μm(200目)的筛并于160℃烘干1 h,称取50 mg样品,置于镍坩埚中,加入1.5 g氢氧化钾,以650℃高温熔融,冷却后用稀硝酸浸取熔融物,用水定容至200 mL。采用Burgener雾化器提高雾化效率,以钾盐进行基体匹配,以元素钇作为内标进行定量。硅(硼)的质量浓度与硅(硼)元素和内标元素的谱线强度比具有良好的线性关系,硅元素的检出限为0.0004 mg/mL,硼元素的检出限为0.00006 mg/mL。硅、硼元素测定结果的相对标准偏差均不大于1.0%(n=6),实际样品加标回收率为95.1%~97.1%。该方法硅、硼的测定结果与GJB 1679A—2008《高硅氧玻璃纤维纱规范》中二氧化硅含量测试方法和JB/T 7993—1999《碳化硼化学分析方法》中总硼含量的测试方法的测定结果一致。该方法适用于批量样品的检测。A method was established for the determination of silicon and boron elements in Si-B-C-N ceramics by inductively coupled plasma atom emission spectrometry(ICP-AES).The sample was crushed to through a 75μm seive and dried at 160℃for 1 h.50 mg sample was weighed and melt in 650℃with 1.5 g potassium hydroxide in a nickel crucible.After the crucible was taken out and cooled,molten material was dissolved with dilute nitric acid and the solution was transferred to a 200 mL volumetric flask and diluted to 200 mL with water.The Burgener nebulizer was used to improve atomization efficiency,potassium salt was used for matrix matching,and element yttrium was used as the internal standard for quantification.The mass concentration of silicon(boron)had a good linear relationship with the spectral line intensity ratio of silicon(boron)element and internal standard element.The detection limit of silicon element was 0.0004 mg/mL,and the detection limit of boron element was 0.00006 mg/mL.The relative standard deviations of silicon and boron determination results were less than 1.0%(n=6),and the recoveries were 95.1%-97.1%.The determination results of silicon and boron by this method were consistent with the determination results of Si content in GJB 1679A—2008"Specification for High Silica Glass Fiber Yarn"and the determination results of total boron content in JB/T 7993—1999"Method for Chemical Analysis of Boron Carbide".This method is suitable for the detection of batch samples.

关 键 词：硅硼碳氮陶瓷产品 电感耦合等离子体原子发射光谱法 硅 硼 

分 类 号：O657.3[理学—分析化学]