熔融制样-X射线荧光光谱法测定稀土硅铁中11种主次元素  

Determination of 11 major and minor elements in rare earth ferrosilicon by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：万芒 刘伟[2] 曾小平 WAN Mang;LIU Wei;ZENG Xiaoping(Analytical&Testing Center,South China University of Technology,Guangzhou 510641,China;Technology Center of Shanxi Taigang Stainless Steel Co.,Ltd.,Taiyuan 030003,China)

机构地区：[1]华南理工大学分析测试中心,广东广州510641 [2]山西太钢不锈钢股份有限公司技术中心,山西太原030003

出　　处：《冶金分析》2023年第1期54-61,共8页Metallurgical Analysis

摘　　要：采用X射线荧光光谱法(XRF)测定稀土硅铁中硅、锰、铝、铁、钛及镧系元素时,熔融制样过程中氧化条件不好控制,容易造成挂壁坩埚过早熔化或坩埚挂壁不好的现象,使铂-金坩埚受到严重侵蚀。实验以四硼酸锂为熔剂铺底保护铂-金坩埚,使用碳酸锂对稀土硅铁样品进行烧结氧化;再采用过氧化钠进行深度氧化,解决了稀土硅铁合金对铂-金坩埚腐蚀的问题。试样和四硼酸锂熔剂的质量比为1∶30,在1100℃下熔融试样12 min,可制得表面质量良好的玻璃片,有效地消除了试样的粒度效应和矿物效应影响。按照实验方法测定稀土硅铁中硅、锰、铝、钙、铁、钛、镧、铈、镨、钕、钐等11种主次元素,结果的相对标准偏差(RSD,n=10)为0.39%~5.0%,与标准方法及滴定法分析结果吻合较好,能满足稀土硅铁中主次元素的检测需求。During the determination of silicon,manganese,aluminum,iron,titanium and lanthanide-series elements in rare earth ferrosilicon by X-ray fluorescence spectrometry(XRF),the oxidation conditions in the process of fusion sample preparation are not easily controlled.It is easy to cause the phenomenon of premature melting of the wall hanging crucible or poor wall hanging of the crucible,which will seriously erode the platinum-gold crucible.In the experiment,lithium tetraborate was used as the flux on the bottom of platinum-gold crucible for protection.The rare earth ferrosilicon samples were sintered and oxidized with lithium carbonate.Then sodium peroxide was used for deep oxidation,which solved the corrosion problem of platinum-gold crucible by rare earth ferrosilicon sample.The mass ratio of sample to lithium tetraborate flux was 1∶30.After fusion at 1100℃for 12 min,the prepared glass sheets had good surface quality,which effectively eliminated the influence of grain-size effect and mineral effect.11 major and minor elements(including silicon,manganese,aluminum,calcium,iron,titanium,lanthanum,cerium,praseodymium,neodymium and samarium)in rare earth ferrosilicon were determined according to the experimental method.The relative standard deviations(RSD,n=10)of the determination results were between 0.39%and 5.0%,and the results were in good agreement with those obtained by standard method and titration method.The proposed method could meet the detection requirements of the major and minor elements in rare earth ferrosilicon.

关 键 词：预氧化 熔融制样 X射线荧光光谱法(XRF) 稀土硅铁 稀土 

分 类 号：O657.34[理学—分析化学] TF031[理学—化学] TF645[冶金工程—冶金物理化学]