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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 被引量:7

XRFS Determination of Boron, Silicon, Aluminum and Phosphorus in Ferroboron Alloy with Pre-Oxidation Fusion Sample Preparation
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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.
作者 宋祖峰 陆向东 陈海峰 荚江霞 王忠乐 郭士光 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)
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2019年第5期545-549,共5页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词 X射线荧光光谱法 预氧化 熔融制样 硼铁合金 XRFS pre-oxidation fusion sample preparation B Si Al P ferroboron alloy
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