GD-MS用高纯钼成分分析质量控制样品的研制  

Manufacturing of Quality Control Samples for Composition Analysis of High Purity Molybdenum by GD-MS

作　　者：王焕文 陈雄飞 孙泽明 贾国斌[1,2] 童坚 Wang Huanwen;Chen Xiongfei;Sun Zeming;Jia Guobin;Tong Jian(National Analysis and Testing Center of Nonferrous Metals and Electronic Materials,GRINM Group Co.,Ltd.,China United Test&Certifaation Co.,Ltd.,Beijing WQQ88,China;General Research Institute for Nonferrous Metals,Beijing 100088,China)

机构地区：[1]有研科技集团有限公司国家有色金属及电子材料分析测试中心,国合通用评价测试认证股份有限公司,北京100088 [2]北京有色金属研究总院,北京100088

出　　处：《稀有金属》2022年第1期131-136,共6页Chinese Journal of Rare Metals

基　　金：国家重点研发计划项目(2017YFB0305400)资助。

摘　　要：辉光放电质谱(GD-MS)是目前常用的高纯金属化学成分检测手段之一,然而使用GD-MS对高纯金属中的杂质含量进行定量分析时,需要与基体匹配的成分分析质控样品对相对灵敏度因子(RSF)进行校正。以钼酸铵和金属盐溶液为原料,采用液相掺杂,搅拌加热,蒸发结晶的方法得到掺杂钼酸铵。经氢化还原后,采用机械搅拌方式进一步进行均匀化处理,成功制备了GD-MS用高纯钼成分分析质控样品。考察了制备过程中均匀化处理时间对样品粒度分布,微观形貌及对样品杂质含量均匀性的影响。使用电感耦合等离子体质谱(ICP-MS)对本质控样品进行检测,经方差齐性检验,质控样品中杂质元素的含量均匀性达标。使用本质控样品对高纯钼中的Al,Fe,Cr,Co,Ni,Sb,Hf等7种元素的GD-MSRSF值进行校正,用于高纯钼样品检测。经平均值一致性检验,GD-MS测定值与ICP-MS测定结果一致。方法的相对标准偏差(RSD)为0.53%~2.26%。With the development of molybdenum metallurgical industry,investigators had more stringent requirements for precision and accuracy in their detection methods of high-purity molybdenum.Glow discharge mass spectrometry(GD-MS)was one of the commonly used chemical composition detection means for high-purity metals.However,when using GD-MS to quantitatively analyze the impurity content in high-purity metals,composition analysis with matrix matched quality control samples was required to correct the relative sensitivity factor(RSF).GD-MS could only analyze the composition of bulk solid samples.Therefore,the general molybdenum standard solution could not be used to correct the relative sensitivity factor of molybdenum.The most commonly used method for preparing standard solid metal samples was smelting mixing,in which the matrix elements and impurity metals were melted and fully mixed to homogenize the impurity elements.The melting point of molybdenum was up to 2610℃.Therefore,there was no suitable high-temperature vessel for mixing melted molybdenum with other pure metals.Solid quality control samples could also be prepared by mixing the standard solution in a certain proportion and steaming it dry.Liquid phase mixing was easier to achieve homogenization of impurities in quality control samples.However,this method was expensive,and the inorganic salt solution would be hydrolyzed during evaporation.In order to solve the above problems,a preparation method of high purity molybdenum standard solid sample for composition analysis was developed.In this paper,ammonium molybdate and metal salt solution containing required impurities were mixed,stirred and evaporated for crystallization at 150℃for 24 h.After preliminary homogenization,crude ammonium molybdate crystal with uniform composition was obtained.High purity doped molybdenum powder was prepared by hydrogenation reduction of ammonium molybdate(reduction temperature of 900℃,hydrogen flow of 15~20 L·h^(-1)).The quality control sample of high purity molybdenum for G

关 键 词：辉光放电质谱 高纯钼 多元素掺杂 均匀化 质控样品 

分 类 号：O657.63[理学—分析化学]