Abstract：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 53 μm (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, 0.000 99% for Al, 0.001 9% for Si, 0.000 72% for P, 0.000 41% for S, 0.003 4% for Ti, and 0.003 9% 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.
[1] LIN Yinghua,LI Hui,JU Jiang,et al.Effect of boron content on high-temperature oxidation resistance of B-bearing high-speed steel[J].Surface Review and Letters,2020,27(12):2050023. [2] 宋祖峰,陆向东,陈海峰,等.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[J].理化检验(化学分册),2019,59(5):545-549. SONG Zufeng,LU Xiangdong,CHEN Haifeng,et al.XRFS determination of boron,silicon,aluminum and phosphorus in ferroboron alloy with pre-oxidation fusion sample preparation[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis),2019,59(5):545-549. [3] 国家技术监督局.GB/T 3653.1-1988 硼铁化学分析方法 碱量滴定法测定硼量[S].北京:中国标准出版社,1988. [4] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 3653.4-2008 硼铁 铝含量的测定 EDTA滴定法[S].北京:中国标准出版社,2008. [5] 国家技术监督局.GB/T 3653.3-1988 硼铁化学分析方法 高氯酸脱水重量法测定硅量[S].北京:中国标准出版社,1988. [6] 中华人民共和国冶金工业部.GB/T 3653.6-1988 硼铁化学分析方法 锑磷钼蓝光度法测定磷量[S].北京:中国标准出版社,1988. [7] 国家市场监督管理总局;国家标准化管理委员会.GB/T 3653.7-2020 硼铁 硫含量的测定 红外线吸收法[S].北京:中国标准出版社,2020. [8] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 6730.63-2006 铁矿石 铝、钙、镁、锰、磷、硅和钛含量的测定 电感耦合等离子体发射光谱法[S].北京:中国标准出版社,2006. [9] 张涛,陈朝阳,陈景伟.粉末压片-能量色散X射线荧光光谱法测定多金属矿石中锡[J].冶金分析,2023,43(2):23-30. ZHANG Tao,CHEN Zhaoyang,CHEN Jingwei.Determination of tin in polymetallic ore by energy dispersive X-ray fluorescence spectrometry with powder pellet preparation[J].Metallurgical Analysis,2023,43(2):23-30. [10] 刘洪涛,邵常丽.能量色散X射线荧光光谱法测定铁矿石中化学成分[J].冶金分析,2016,36(6):69-72. LIU Hongtao,SHAO Changli.Determination of chemical components in iron ores by energy dispersive X-ray fluorescence spectrometry[J].Metallurgical Analysis,2016,36(6):69-72. [11] 张永顺,孙雪涛,袁辉,等.压片制样-X射线荧光光谱法分析铁矿石中钾钠锌[J].冶金分析,2019,39(1):72-76. ZHANG Yongshun,SUN Xuetao,YUAN Hui,et al.Determination of potassium,sodium and zinc in iron ore by X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis,2019,39(1):72-76. [12] 仵利萍,刘卫.X射线荧光光谱法测定铁矿石的化学成分[J].矿产综合利用,2010(3):42-45. WU Liping,LIU Wei.Determination of chemical composition of iron ores by X-ray fluorescence spectrographic method[J].Multipurpose Utilization of Mineral Resources,2010(3):42-45. [13] 单华珍,卓尚军,盛成,等.粉末压片法波长色散X射线荧光光谱分析铁矿石样品的矿物效应校正初探[J].光谱学与光谱分析,2008,28(7):1661-1664. SHAN Huazhen,ZHUO Shangjun,SHENG Cheng,et al.Mineralogical effect correction for pressed iron ore samples in wavelength dispersive X-ray fluorescence analysis[J].Spectroscopy and Spectral Analysis,2008,28(7):1661-1664. [14] 卜兆杰,蒋春宏,陶泽秀,等.粉末压片制样-X射线荧光光谱法测定稀土镁中间合金中镁锰硅钛钙铁[J].冶金分析,2018,38(3):61-64. BU Zhaojie,JIANG Chunhong,TAO Zexiu,et al.Determination of magnesium,manganese,silicon,titanium,calcium,iron in rare-magnesium intermediate alloy by X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis,2018,38(3):61-64. [15] 阿丽莉,贺攀红,张盼盼.粉末压片-X射线荧光光谱法测定地质样品中镧铈镨钕钐[J].冶金分析,2019,39(9):39-45. A Lili,HE Panhong,ZHANG Panpan.Determination of lanthanum,cerium,praseodymium,neodymium and samarium in geological sample by X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis,2019,39(3):39-45. [16] 兰福荫,蒙文飞,刘杰,等.粉末压片-能量色散X射线荧光光谱法测定粗制氢氧化钴中钴铜铁锰钙镁铝[J].冶金分析,2024,44(3):30-35. LAN Fuyin,MENG Wenfei,LIU Jie,et al.Determination of cobalt,copper,iron,manganese,calcium,magnesium and aluminum in crude cobalt hydroxide by energy dispersive X-ray fluorescence spectrometry with powder pellet preparation[J].Metallurgical Analysis,2024,44(3):30-35.
