Determination of 8 components in manganese slag by X-ray fluorescence spectrometry with fusion sample preparation
DENG Junhua1,2, KANG Dehua1,2, HU Zhongxin1,2, GAO Pin1,2 WANG Yiling1,2, YANG Jie1,2
1. State Key Laboratory of Metal Material for Marine Equipment and Application,Anshan 114009,China; 2. Iron & Steel Research Institute of Ansteel Group,Anshan 114009,China
Abstract：The determination of components in manganese slag usually adopts chemical wet method with complicated operation.Lithium tetraborate was used as flux.The certified reference materials of slag,manganese-rich slag and manganese ore were selected,and their synthetic calibration samples with different mass ratios were prepared.The calibration sample series with a certain gradient and a wide enough content range were used to draw calibration curves,which overcame the influence of matrix effect.The empirical coefficient method(MC) was used to correct the spectral enhancement-absorption interference among the components in manganese slag.The analysis method for the determination of 8 components in manganese slag,including SiO2,Al2O3,CaO,MgO,TMn,P2O5,TiO2 and TFe,by X-ray fluorescence spectrometry(XRF) was established.Through the optimization of dilution ratio,pre-oxidation method,fusion temperature, fusion time and the dosage of release agent,the problems of nonuniform forming and difficulty in demoulding caused by high viscosity and weak fluidity of molten manganese slag from lithium tetraborate were solved.The results showed that the linear correlation coefficients of calibration curves were higher than 0.999 7,and the limit of detection was 11.2-90.2 μg/g.The experimental method was applied to the determination of each component in manganese slag samples,and the relative standard deviations (RSDs, n=6) of the measured results were between 0.27% and 3.7%. The components in manganese slag samples were determined by the experimental method and standard method,respectively.The results of two methods were basically consistent.
邓军华, 亢德华, 胡忠新, 高品, 王一凌, 杨洁. 熔融制样-X射线荧光光谱法测定锰渣中8种组分[J]. 冶金分析, 2023, 43(7): 96-101.
DENG Junhua, KANG Dehua, HU Zhongxin, GAO Pin WANG Yiling, YANG Jie. Determination of 8 components in manganese slag by X-ray fluorescence spectrometry with fusion sample preparation. , 2023, 43(7): 96-101.
[1] 万维华,范翔,史磊.浅谈电解二氧化锰渣的资源化利用[J].中国资源综合利用,2020,38(2):57-59. WAN Weihua,FAN Xiang,SHI Lei.Brief introduction of the resource utilization of electrolytic manganese dioxide slag[J].China Resources Comprehensive Utilization,2020,38(2):57-59. [2] 车丽诗,雷鸣.锰渣资源化利用的研究进展[J].中国锰业,2016,34(3):128-130. CHE Lishi,LEI Ming.Research of resource utilization of manganese residue[J].China's Manganese Industry,2016,34(3):128-130. [3] 刘琼鲜,杨睿瑶,杨满洲,等.碱熔-电感耦合等离子体原子发射光谱法测定钒铁炉渣中钒铁锰磷[J].矿产综合利用,2022(3):207-210. LIU Qiongxian,YANG Ruiyao,YANG Manzhou,et al.Determination of vanadium,iron,manganese and phosphorus contents in ferrovanadium slag by alkali fusion-inductively coupled plasma atomic emission spectrometry[J].Multipurpose Utilization of Mineral Resources,2022(3):207-210. [4] 成勇,刘力维,袁金红,等.碱熔-电感耦合等离子体原子发射光谱法测定钒渣中钒硅钙镁铝锰铬钛磷[J].冶金分析,2021,41(4):59-67. CHENG Yong,LIU Liwei,YUAN Jinhong,et al.Determination of vanadium,silicon,magnesium,aluminum,manganese,chromium,titanium and phosphorus in vanadium slag by inductively coupled plasma atomic emission spectrometry after alkali fusion[J].Metallurgical Analysis,2021,41(4):59-67. [5] 成勇.电感耦合等离子体原子发射光谱法测定高钛渣铁中锰磷钒[J].冶金分析,2005,25(6):58-61. CHENG Yong.Determination of manganese,phosphorus and vanadium in the iron slag with high content titanium by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2005,25(6):58-61. [6] 刘洪泉,陈娟.火焰原子吸收光度法测定高钛渣中的锰铬[J].云南冶金,2018,47(1):63-67. LIU Hongquan,CHEN Juan.The determination of manganese,chromium in high titanium slag by flame atomic absorption spectrum[J].Yunnan Metallurgy,2018,47(1):63-67. [7] 张穗忠,邵梅,李杰,等.原子吸收光谱法测定保护渣中锰含量[J].武钢技术,2015,53(2):24-25. ZHANG Suizhong,SHAO Mei,LI Jie,et al.Determination of manganese in mold fluxes by atomic absorption spectroscopy[J].Wisco Technology,2015,53(2):24-25. [8] 王小强,程宝成,张磊,等.硫酸亚铁铵滴定法测定锰渣中的锰含量[J].中国无机分析化学,2020,10(5):19-23. WANG Xiaoqiang,CHENG Baocheng,ZHANG Lei,et al.Determination of manganese in manganese slag by ammonium ferrous sulfate titration[J].Chinese Journal of Inorganic Analytical Chemistry,2020,10(5):19-23. [9] 郝鹏,郑利,赵斌.碱熔测定中锰渣中氧化钙含量[J].铁合金,2020,51(5):46-48. HAO Peng,ZHENG Li,ZHAO Bin.Determination of calcium oxide in medium carbon ferromanganese slag by alkaline fusion[J].Ferro-Alloys,2020,51(5):46-48. [10] 傅伟东,黄静,黄伟光,等.锰渣中三氧化二铝的快速测定[J].冶金分析,2002,22(2):70-72. FU Weidong,HUANG Jing,HUANG Weiguang,et al.Rapid determination of aluminiun oxide in manganese slag[J].Metallurgical Analysis,2002,22(2):70-72. [11] 中华人民共和国工业和信息化部.YB/T 140—2009 钢渣化学分析方法[S].北京:冶金工业出版社,2010. [12] 中华人民共和国工业和信息化部.YB/T 190.13—2014 连铸保护渣 二氧化硅、三氧化二铝、氧化钙、氧化镁、全铁含量的测定 波长色散X射线荧光光谱法[S].北京:冶金工业出版社,2015. [13] 中华人民共和国国家发展和改革委员会.YB/T 4177—2008 炉渣X射线荧光光谱分析方法[S].北京:冶金工业出版社,2008. [14] 张祥,陆晓明,金德龙,等.熔融制样-X射线荧光光谱测定不锈钢渣中10种组分[J].冶金分析,2016,36(1):40-44. ZHANG Xiang,LU Xiaoming,JIN Delong,et al.Determination of ten components in stainless steel slag by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2016,36(1):40-44.
