预氧化熔融制样-X射线荧光光谱法测定硼铁合金中硼、硅、铝和磷  

XRFS Determination of Boron, Silicon, Aluminum and Phosphorus in Ferroboron Alloy with Pre-Oxidation Fusion Sample Preparation

作　　者：宋祖峰 陆向东[3] 陈海峰[3] 荚江霞[2] 王忠乐[2] 郭士光[2] 贾云海 SONG Zufeng;LU Xiangdong;CHEN Haifeng;JIA Jiangxia;WANG Zhongle;GUO Shiguang;JIA Yunhai(Central Iron and Steel Research Institute,Beijing 100081,China;Technology Center of Maanshan Iron and Steel Co.,Ltd.,Ma' anshan 243000,China;Jiangsu Yonggang Group Co.,Ltd.,Zhang jiagang 215628,China)

机构地区：[1]钢铁研究总院,北京100081 [2]马鞍山钢铁股份有限公司技术中心,马鞍山243000 [3]江苏永钢集团有限公司,张家港215628

出　　处：《理化检验（化学分册）》2019年第5期545-549,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：硼铁合金样品经过预氧化熔融,制得样品的玻璃熔片,采用X射线荧光光谱法测定玻璃熔片中硼、硅、铝和磷等4种元素的含量。优化的试验条件如下:(1)熔剂为焦硫酸钾;(2)熔剂与样品的稀释比为40∶1;(3)氧化剂为碳酸锂和硝酸钠;(4)玻璃熔片的熔融时间为20min。4种元素的质量分数在一定范围内与其对应的荧光强度呈线性关系,测定下限为0.006 8%～0.017 9%。对硼铁标准样品平行测定10次,测定值的相对标准偏差为0.22%～3.9%。方法应用于硼铁合金样品的分析,测定结果与湿法分析的结果相符。The ferroboron alloy sample was melted with pre-oxidation fusion,and glass melt of the sample was prepared.XRFS was applied to the determination of 4 elements, i.e.boron,silicon,aluminum and phosphorus in the glass melt.The optimized conditions found were as follows:(1) the flux was potassium pyrosulfate;(2) the dilution ratio of flux to sample was 40∶1;(3)lithium carbonate and sodium nitrate were used as the oxidant;(4) the melting time of glass melt was 20 minutes.Linear relationships between values of fluorescence intensity and mass fraction of the 4 elements were kept in definite ranges,with lower limits of determination in the range of 0.006 8%-0.017 9%.Ferroboron standard sample was tested for 10 determinations,values of RSDs of determination values were in the range of 0.22%-3.9%.The proposed method was applied to the analysis of ferroboron alloy sample,giving results in consistency with the values obtained by wet process.

关 键 词：X射线荧光光谱法 预氧化 熔融制样 硼 硅 铝 磷 硼铁合金 

分 类 号：O657.34[理学—分析化学]