Quantitative determination of 4 phases in iron oxide scale by mass absorption coefficient modification-X-ray diffraction external standard method
QIAO Zhu1, WANG Heng1, SU Mingyue2, ZHAO Xiurong1, ZHANG Pingping1, WANG Yonghong3
1. Comprehensive Technology Center of Lianyungang Customs,Lianyungang 222042,China; 2. Industrial Product Safety Technology Center of Tianjin Customs,Tianjin 300456,China; 3. Institute of Research of Iron ＆ Steel,Sha-steel,Jiangsu Province,Zhangjiagang 215625,China
Abstract：The accurate and quantitative analysis of phase of iron oxide scale can provide important parameters for the control,elimination and reuse of iron oxide scale.An improved X-ray diffraction(XRD) external standard method for quantitative analysis of phase content in iron oxide scale was established in experiments.The mass absorption coefficients were calculated by the elemental contents in sample.The calibration curves were established using the phase content as the horizontal coordinate,and the product of phase diffraction intensity and sample mass absorption coefficient as the vertical coordinate.The simultaneous quantification of Fe2O3,Fe3O4,FeO and SiO2 was realized.The sample preparation,scanning conditions and integration methods were investigated.The sample size was 45 μm or less,the scanning step was 0.01°,the time per step was 30 s,and the integral was based on peak area.Under the selected conditions,the determination coefficient(R2) of calibration curve of each phase was 0.998 8-0.999 3,and the limit of detection(LOD) was 1.1%-4.2%.The iron oxide scale samples of rolled and continuous casting were determined.The relative standard deviations(RSD,n=6) were between 2.3% and 10.2%,the recoveries were between 92% and 110%.The proposed method was compared with X-ray full spectrum fitting method,and the results were consistent.It was suitable for the determination of amorphous samples,and it could meet the requirements of precise quantitative analysis of phases in the iron oxide scale.
乔柱, 王恒, 苏明跃, 赵秀荣, 张萍萍, 王永红. 质量吸收系数修正-X射线衍射外标法定量分析氧化铁皮中4种物相[J]. 冶金分析, 2024, 44(7): 55-61.
QIAO Zhu, WANG Heng, SU Mingyue, ZHAO Xiurong, ZHANG Pingping, WANG Yonghong. Quantitative determination of 4 phases in iron oxide scale by mass absorption coefficient modification-X-ray diffraction external standard method. , 2024, 44(7): 55-61.
[1] 张迪,郭云侠,于帅,等.中厚板精轧过程中除鳞工艺对氧化铁皮结构的影响[J].安徽工业大学学报(自然科学版),2021,38(1):18-23. ZHANG Di,GUO Yunxia,YU Shuai,et al.Effect of descaling process on the structure of oxide scale during the finishing rolling of medium and heavy plates[J].Journal of Anhui University of Technology(Natural Science),2021,38(1):18-23. [2] Bhattacharya R,Jha G,Kundu R,et al.Influence of cooling rate on the structure and formation of oxide scale in low carbon steel wire rods during hot rolling[J].Surface and Coatings Technology,2016,201:526. [3] 林冲,刘宏玉,王宏军,等.帘线钢等温和控冷过程氧化铁皮的形成[J].钢铁研究学报,2015,27(6):40-44,50. LIN Chong,LIU Hongyu,WANG Hongjun,et al.Formation of oxide scale on tire cord steel during isothermal holding and controlled cooling[J].Journal of Iron and Steel Research,2015,27(6):40-44,50. [4] 林飞,王春峰,李志峰,等.酸洗工艺对热轧酸洗板表面质量影响机理研究[J].轧钢,2019,36(2):11-18. LIN Fei,WANG Chunfeng,LI Zhifeng,et al.Study on the effect mechanism of pickling process on surface quality of hot rolled pickling plate[J].Steel Rolling,2019,36(2):11-18. [5] SEN R,PANDEL U.Closed crucible reduction of lump powdered mill scale or iron ore by coal:The sequential methodology and mechanism for optimization of process parameters[J].Advanced Powder Technology,2020,31(9):3760-3773. [6] 权淑丽,王炜.X射线衍射法测定热轧带钢氧化皮中相的含量[J].物理测试,2015,33(2):22-25. QUAN Shuli,WANG Wei.Determination of content of phase of hot-rolled strip oxide scale by X-ray diffraction[J].Physics Examination and Testing,2015,33(2):22-25. [7] 陈兴润,潘吉祥,纪显彬,等.S32101双相不锈钢热轧中厚板氧化铁皮显微分析[J].钢铁研究学报,2021,33(1):84-89. CHEN Xingrun,PAN Jixiang,JI Xianbin,et al.Analysis of oxide scales microstructure of hot-rolled plate in S32101 duplex stainless steel[J].Journal of Iron and Steel Research,2021,33(1):84-89. [8] 张春花,田秀刚,藏振东,等.用显微镜观察氧化铁皮分层结构的方法[J].特钢技术,2023,29(2):51-54,58. ZHANG Chunhua,TIAN Xiugang,ZANG Zhendong,et al.Method for observing the layered structure of iron oxide scale with a microscope special[J].Steel Technology,2023,29(2):51-54,58. [9] 乔柱,郑建明,宋见峰,等. Si内标-X射线衍射法定量测定铁矿中Fe3O4、Fe2O3和SiO2[J].中国无机分析化学,2023,13(5):463-468. QIAO Zhu,ZHENG Jianming,SONG Jianfeng,et al.Quantitative determination of Fe3O4,Fe2O3and SiO2in iron ore by Si internal standard-X-ray diffraction method[J].Chinese Journal of Inorganic Analytical Chemistry,2023,13(5):463-468. [10] 王超,余嘉栋,王震威,等.具有疑似爆炸性的未知复杂样品分析方法研究[J].分析试验室,2016,35(1):34-37. WANG Chao,YU Jiadong,WANG Zhenwei,et al.Analysis methods on unknown complex samples containing suspected explosives[J].Chinese Journal of Analysis Laboratory,2016,35(1):34-37. [11] 周君龙,陈宜浩,李全忠,等. X射线衍射Rietveld全谱拟合法定量检测滑石混合矿物中滑石含量 [J].冶金分析,2023,43(4):18-23. ZHOU Junlong,CHEN Yihao,LI Quanzhong,et al.Quantitative determination of talc in talc mixed ore by X-ray diffraction Rietveld full spectrum fitting method[J].Metallurgical Analysis,2023,43(4):18-23. [12] 丁浩.全谱拟合Rietveld法定量分析工业水泥熟料中玻璃体含量的初探[J].水泥,2017(4):63-65. DING Hao.Preliminary study on quantitative analysis of vitreous content in industrial cement clinker by Rietveld refinement method[J].Cement,2017(4):63-65. [13] 冉敬,杜谷,王凤玉.X射线衍射全谱拟合法快速分析长石矿物含量[J].岩矿测试,2017,36(5):489-494,449. RAN Jing,DU Gu,WANG Fengyu.Rapid analysis of feldspar by X-ray diffractometry Rietveld refinement method[J].Rock and Mineral Analysis,2017,36(5):489-494,449. [14] 吴建鹏,曹丽云,黄剑锋,等.无机材料中24种组分X射线衍射物相定量分析外标法标准曲线库的建立[J].岩矿测试,2007,26(5):398-400. WU Jianpeng,CAO Liyun,HUANG Jianfeng,et al.Foundation of the standard curve database for quantitative phase analysis of 24 components in inorganic materials by X-ray diffractometry based on external standard method[J].Rock and Mineral Analysis,2007,26(5):398-400. [15] 黄继武,李周.多晶材料X射线衍射-实验原理方法与应用[M].2版.北京:冶金工业出版社,2021. [16] 卞欣.X射线衍射仪在氧化铁皮物相分析中的应用[J].现代冶金,2013,41(6):12-15. BIAN Xin.Application of X-ray diffractometer in phase analysis of oxidized iron sheet[J].Modern Metallurgy,2013,41(6):12-15.
