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  

Quantitative determination of 4 phases in iron oxide scale by mass absorption coefficient modification-X-ray diffraction external standard method

作　　者：乔柱 王恒 苏明跃 赵秀荣 张萍萍 王永红 QIAO Zhu;WANG Heng;SU Mingyue;ZHAO Xiurong;ZHANG Pingping;WANG Yonghong(Comprehensive Technology Center of Lianyungang Customs,Lianyungang 222042,China;Industrial Product Safety Technology Center of Tianjin Customs,Tianjin 300456,China;Institute of Research of Iron&Steel,Sha-steel,Jiangsu Province,Zhangjiagang 215625,China)

机构地区：[1]连云港海关综合技术中心,江苏连云港222042 [2]天津海关工业产品安全技术中心,天津300456 [3]江苏省(沙钢)钢铁研究院有限公司,江苏张家港215625

出　　处：《冶金分析》2024年第7期55-61,共7页Metallurgical Analysis

基　　金：连云港市重点研发计划(SF2223);海关总署科技项目(2023HK111)。

摘　　要：氧化铁皮物相的准确定量分析可以为氧化铁皮的控制、消除以及再利用工艺提供重要参数。实验建立了一种改进的X射线衍射(XRD)外标定量分析氧化铁皮中物相含量的方法,通过样品元素含量计算出质量吸收系数,以物相含量为横坐标,衍射峰强度与质量吸收系数乘积为纵坐标建立校准曲线,实现了对Fe_(2)O_(3)、Fe_(3)O_(4)、FeO和SiO_(2)物相的同时定量。试验对制样、扫描条件和积分方式进行了考察,样品粒度不大于45μm,扫描步长0.01°,步时30 s,以峰面积积分。在选定条件下各物相校准曲线的决定系数(R2)为0.9988~0.9993,检出限(LOD)为1.1%~4.2%。选取轧钢氧化铁皮和连铸氧化铁皮样品进行了测定,相对标准偏差(RSD,n=6)为2.3%~10.2%,加标回收率为92%~110%。方法与X射线全谱拟合法进行了对比,结果一致。方法适用于含非晶相样品的测定,满足氧化铁皮中物相的精确定量分析要求。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 Fe_(2)O_(3),Fe_(3)O_(4),FeO and SiO_(2) was realized.The sample preparation,scanning conditions and integration methods were investigated.The sample size was 45μm 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(R^(2))of calibration curve of each phase was 0.9988-0.9993,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.

关 键 词：氧化铁皮 X射线衍射(XRD) 外标法 质量吸收系数 三氧化二铁 四氧化三铁 氧化亚铁 二氧化硅 非晶相 

分 类 号：O72[理学—晶体学] TF042[冶金工程—冶金物理化学]