粉末压片-X射线荧光光谱法测定硼铁中多元素  

Determination of multi-elements in ferroboron by X-ray fluorescence spectrometry with powder pellet preparation

作　　者：聂成宏 吴文琪[1] 任旭东[1] 李欣欣 郭向喜 孔令娟 NIE Chenghong;WU Wenqi;REN Xudong;LI Xinxin;GUO Xiangxi;KONG Lingjuan(Baotou Research Institute of Rare Earth,Baotou 014030,China;Inner Mongolia Yonglei Material Technology Co.,Ltd.,Baotou 014070,China)

机构地区：[1]包头稀土研究院,内蒙古包头014030 [2]内蒙古永磊材料科技有限公司,内蒙古包头014070

出　　处：《冶金分析》2024年第9期58-65,共8页Metallurgical Analysis

摘　　要：准确快速测定硼铁合金中硼及杂质元素的含量,对科学指导炼铁炼钢生产,保证高附加值钢铁的质量起着至关重要的作用。本文采用粉末压片制样,选用2个硼铁标准物质及国标法定值的硼铁样品组成各元素含量具有一定梯度且含量跨度能够覆盖样品中各元素含量范围的校准样品系列绘制校准曲线以克服基体效应,实现了X射线荧光光谱法对硼铁中B、Al、Si、P、S、Ti、Mn的测定。对制样条件进行了优化,确定采用1.50 g粒度为53μm(过280目筛)的样品,以硼酸镶边垫底于44 MPa保压40 s制成样片;采用经验系数法浓度校正方式校正了B的基体效应。方法检出限为B 0.085%,Al 0.00099%,Si 0.0019%,P 0.00072%,S 0.00041%,Ti 0.0034%,Mn 0.0039%。应用实验方法将硼铁样品平行压制成6个不同样片进行测定,各元素测得结果的相对标准偏差(RSD)均小于2.0%。按照实验方法测定硼铁样品,测定结果分别与GB/T 3653.1—1988中碱量滴定法测定B,GB/T 3653.4—1988中EDTA滴定法测定Al,GB/T 3653.3—1988中高氯酸脱水重量法测定Si,GB/T 3653.6—1988中锑磷钼蓝分光光度法测定P,GB/T 3653.7—2020中红外线吸收法测定S,GB/T 6730.63—2006中的电感耦合等离子体原子发射光谱法测定Ti和Mn的结果基本一致。Accurate and rapid determination of boron and impurities in ferroboron is of great importance for the scientific guidance of ironmaking and steelmaking production as well as ensuring the quality of high value-added steel.In this study,the sample was prepared by powder pressed pellet.The calibration sample series,which had a certain gradient and a certain content span covering the content ranges of elements in the sample,were prepared with 2 ferroboron certified reference materials and ferroboron samples determined by national standard method to overcome the matrix effect.Thus,the determination of B,Al,Si,P,S,Ti and Mn in ferroboron was realized by X-ray fluorescence spectrometry(XRF).The sample preparation conditions were optimized:1.50 g of sample with particle size of 53μm(screened with 280 mesh)was edged with boric acid and then pressed at 44 MPa for 40 s.The matrix effect of boron was corrected by concentration correction with empirical coefficient method.The limits of detection were listed as below:0.085%for B,0.00099%for Al,0.0019%for Si,0.00072%for P,0.00041%for S,0.0034%for Ti,and 0.0039%for Mn.The proposed method was applied for the determination of 6 different pellets which were parallelly prepared with ferroboron samples.The relative standard deviations(RSD)of determination results of elements were all less than 2.0%.The ferroboron samples were determined according to the proposed method,and the results were basically consistent with those obtained by other methods:B was determined by alkalimetry in GB/T 3653.1-1988;Al was determined by EDTA titration method in GB/T 3653.4-1988;Si was determined by perchloric acid dehydration gravimetry in GB/T 3653.3-1988;P was determined by antimony phosphomolybdenum blue spectrophotometry in GB/T 3653.6-1988;S was determined by infrared absorption method in GB/T 3653.7-2020;Ti and Mn were determined by inductively coupled plasma-atomic emission spectrometry in GB/T 6730.63-2006.

关 键 词：X射线荧光光谱法(XRF) 粉末压片 硼铁 硼 

分 类 号：O657.34[理学—分析化学] TF64[理学—化学]