硅钼蓝分光光度法测定氮化硼中Si含量  

Determination of silicon content in boron nitride by silicon molybdenum blue spectrophotometry

作　　者：李涛 张力久 栗生辰 王长华 李蒙 邓楠 李娜 朱冬霞 LI Tao;ZHANG Lijiu;LI Shengchen;WANG Changhua;DENG Nan;LI Meng;LI Na;Zhu Dongxia(Guobiao(Beijing)Testing&Certification Co.,Ltd.,Beijing 101400,China;Youke Publishing Co.,Ltd.,Beijing 100088,China;Shanghai Nonferrous Metals Industry Technology Monitoring Center Co.,Ltd.,Shanghai 200431,China)

机构地区：[1]国标(北京)检验认证有限公司,北京101400 [2]有科期刊出版(北京)有限公司,北京100088 [3]上海有色金属工业技术检测中心有限公司,上海200431

出　　处：《分析试验室》2022年第8期925-929,共5页Chinese Journal of Analysis Laboratory

基　　金：国家新材料测试评价平台-主中心(TC170A5SU/1);国家新材料测试评价平台-有色金属材料行业中心(TC190H3ZW/2)项目资助。

摘　　要：建立了硅钼蓝分光光度法测定氮化硼(BN)中Si含量。BN样品用NaOH熔解,以草硫混酸为掩蔽剂,(NH_(4))_(2)MoO_(4)为显色剂,抗坏血酸为还原剂将硅钼黄杂多酸还原成硅钼蓝配合物,分光光度法测量,并计算Si含量。本方法Si的检出限为0.0050%,检测结果相对标准偏差均在6%以内,加标回收率在96.0%~102.3%之间,可以作为BN中Si含量测定的常规方法。A method for the determination of Si in BN by silicon molybdenum blue spectrophotometry was established.BN samples were melted by NaOH solution.By using grass sulfur mixed acid as masking agent,(NH_(4))^(2) MoO_(4) as color developing agent and ascorbic acid as reducing agent,silicon molybdenum yellow heteropoly acid was reduced to silicon molybdenum blue complex.The content of Si was measured by spectrophotometry method.The detection limit of Si element was 0.0050%,with the relative standard deviation(RSD)within 6%,and the recovery rates between 96.0%and 102.3%.This method can be conventionally used for the determination of Si content in BN.

关 键 词：硅钼蓝 分光光度法 氮化硼 SI含量 

分 类 号：O657.31[理学—分析化学] X832[理学—化学]