Abstract:The key to the determination of high-arbon ferrochrome by X-ray fluorescence spectrometry lies in the preparation of glass bead. It is necessary to ensure the complete melting of the sample and avoid the etching of platinum-gold crucible. There was no need to prepare additional flux crucible. The lithium tetraborate and boron oxide with appropriate proportion were used for bedding. The sample was mixed uniformly with the oxidant of lithium hydroxide, boron oxide and strontium nitrate, and then covered with lithium tetraborate. The homogeneous glass bead which could meet the determination requirements was obtained by selection of the proper melting program. Total of 13 samples, including 4 high-carbon ferrochrome certified reference materials,7 high-carbon ferrochrome samples with fixed values determined by standard method of GB/T 4699, and 2 synthetic high-carbon ferrochrome samples prepared by mixing high purity iron and high-carbon ferrochrome according to certain mass ratio, were selected to draw the calibration curve. Thus, a method for determination of chromium, silicon, phosphorus and titanium in high-carbon ferrochrome was established by X-ray fluorescence spectrometry (XRF). The linear correlation coefficients were all greater than 0.996. The proposed method was applied to the determination of certified reference materials and actual samples of high-carbon ferrochrome. The results were basically consistent with the standard values for certified reference materials. For the actual samples, the relative standard deviations (RSD, n=5) were between 0.15% and 3.4%, and the results were consistent with those obtained by the standard method of GB/T 4699.
张延新, 李京, 刘斌, 刘政鹏. 熔融制样-X射线荧光光谱法测定高碳铬铁中铬硅磷钛[J]. 冶金分析, 2022, 42(12): 77-82.
ZHANG Yanxin, LI Jing, LIU Bin, LIU Zhengpeng. Determination of chromium,silicon,phosphorus and titanium in high-carbon ferrochrome by X-ray fluorescence spectrometry with fusion sample preparation. , 2022, 42(12): 77-82.
[1] 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 4699—2007 铬铁和硅铬铁合金化学分析方法[S].北京:中国标准出版社,2007. [2] 张瑜,刘伟.熔融制样-X射线荧光光谱法测定含碳锆铝耐火材料中氧化锆、氧化铪和氧化铝[J].冶金分析,2020,40(4):65-69. ZHANG Yu,LIU Wei.Determination of zirconium oxide, hafnium oxide and alumina in carbon-bearing zirconium-aluminum refractory material by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2020,40(4):65-69. [3] 杨新能,李小青,杨大军.X射线荧光光谱法测定含还原剂的炼钢辅料中化学成分[J].冶金分析,2014,34(2):40-43. YANG Xinneng,LI Xiaoqing,YANG Dajun.Determination of chemical composition of steelmaking auxiliary materials containing reducing agents by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2014,34(2):40-43. [4] 仵利萍,曾英,刘卫,等.熔融制样-X射线荧光光谱法测定高钛渣主次量元素[J].矿产综合利用,2017(1):81-84. WU Liping,ZENG Ying,LIU Wei,et al.Determination of major and minor elements in high titanium slag by X-ray fluorescence spectrometry with samples of smelting process[J].Multipurpose Utilization of Mineral Resources,2017(1):81-84. [5] 芦飞,赵小琴,刘爱坤.X射线荧光光谱法在线分析高碳铬镍生铁的方法优化[J].山东冶金,2021,43(6):31-35. LU Fei, ZHAO Xiaoqin,LIU Aikun.Method optimization of online analysis of high carbon chromium nickel pig iron by X-ray fluorescence spectrometry[J].Shandong Metallurgy,2021,43(6):31-35. [6] 梁元,沈学静,易启辉,等.X射线荧光光谱法在线测定稀土冶炼分离过程中钬铒铥镱[J].冶金分析,2016,36(8):1-6. LIANG Yuan,SHEN Xuejing,YI Qihui,et al.On-line determination of holmium, erbium, thulium and ytterbium in rare earth smelting separation process by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2016,36(8):1-6. [7] 王平英,陈鹏飞.X射线荧光光谱法同时测定铬铁中铬、硅、锰和磷的含量[J].理化检验(化学分册),2014,50(8):1024-1026. WANG Pingying,CHEN Pengfei.Determination of chromium,silicon,manganese and phosphorus in ferrochromium by X-ray fluorescence spectrometry[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2014,50(8):1024-1026. [8] 杨新能,李小青,杨大军,等.熔融制样-X射线荧光光谱法测定硅铁中硅磷锰铝钙铬[J].冶金分析,2019,39(10):43-48. YANG Xinneng,LI Xiaoqing,YANG Dajun,et al.Determination of silicon,phosphorus,manganese,aluminum,calcium and chromium in ferrosilicon by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2019,39(10):43-48. [9] 刘伟,曹吉祥,张瑜.熔融制样-X射线荧光光谱法测定钨铁合金中硅锰磷铜钨[J].冶金分析,2019,39(2):46-50. LIU Wei,CAO Jixiang,ZHANG Yu.Determination of silicon,manganese,phosphorus,copper,tungsten in ferrotungsten by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2019,39(2):46-50. [10] 滕广清,鲍希波.X射线荧光光谱法测定冰晶石中成分[J].理化检验(化学分册),2009,45(9):1106-1108. TENG Guangqing,BAO Xibo.Determination of components in cryolite by X-ray fluorescence spectrometry[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2009,45(9):1106-1108. [11] 李京.X射线荧光光谱熔片法同时测定锰铁中锰、硅、磷[J].冶金分析,2011,31(6):51-53. LI Jing.Determination of manganese,silicon and phosphorus in ferromanganese by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2011,31(6):51-53. [12] 吴茂华,胡广峰,王念俊.X射线荧光法测定高碳铬铁中的Cr、Si、P[J].山东冶金,2005,27(4):58-59. WU Maohua,HU Guangfeng,WANG Nianjun.Determination of chromium,silicon and phosphorus in ferrochromium by X-ray fluorescence spectrometry[J].Shandong Metallurgy,2005,27(4):58-59. [13] 邢文青,曾霞,马秀艳,等.熔融制样-X射线荧光光谱法测定铬铁中铬硅磷钛[J].冶金分析,2017,37(9):57-62. XING Wenqing,ZENG Xia,MA Xiuyan,et al.Determination of chromium,silicon,phosphorus and titanium in ferrochromium by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2017,37(9):57-62.