Determination of ten components in magnesia refractory material by X-ray fluorescence spectrometry with empirical coefficient method
SUN Xiao-fei1,YANG Dan-dan2,WEN Meng-xi1,JIA Yun-hai*1
1.Central Iron & Steel Research Institute,Beijing 100081,China; 2.Beijing Research Institute of Chemical Engineering and Metallurgy,Beijing 101149,China
Abstract:In order to meet the testing requirements of various magnesia refractory materials, a fusion sample preparation technique was developed with mixed flux (Li2B4O7-LiBO2-LiBr) under the following conditions: dilution ratio of 1∶10, temperature of 1 050 ℃ and fusion time of 20 min. The contents of ten components in magnesia refractory materials (including MgO, CaO, SiO2, Al2O3, Fe2O3, MnO, P2O5, TiO2, Cr2O3 and K2O) were determined by X-ray fluorescence spectrometry (XRF). The calibration curves were prepared using spectral pure reagents, certified reference materials, synthetic samples by pure reagents and standard solution, and chemically certified materials. The correction was selected to correct the inter-element effects according to the comparison of value of the criteria of empirical calibration method. The calibration curves of each component were fitted well, and the matrix effect in magnesia refractory materials was effectively corrected. The precision tests were performed with magnesia refractory materials. The relative standard deviations (RSD, n=7) were between 0.053% and 3.1%. The accuracy tests were also conducted with standard and unknown samples. The found results were consistent with the certified values and those obtained by wet method.
孙晓飞,杨丹丹,文孟喜,贾云海. 经验系数-X射线荧光光谱法测定镁质耐火材料中10种组分[J]. 冶金分析, 2017, 37(5): 12-18.
SUN Xiao-fei,YANG Dan-dan,WEN Meng-xi,JIA Yun-hai. Determination of ten components in magnesia refractory material by X-ray fluorescence spectrometry with empirical coefficient method. , 2017, 37(5): 12-18.
张香荣,陈洁,张立新.铝质、硅质和镁质耐火材料的X射线荧光光谱快速分析[J].冶金分析,2005,25(1):15-18.ZHANG Xiang-rong,CHEN Jie,ZHANG Li-xin.Rapid analysis of silicon,magnesium and aluminum base refractory materials by XRF[J].Metallurgical Analysis,2005,25(1):15-18.
[3]
宋祖峰,阚斌,陈健.镁铝铬质耐火材料的X射线荧光光谱分析[J].理化检验:化学分册,2005,41(9):648-653.SONG Zu-feng,KAN Bin,CHEN Jian.XRFS analysis of Mg-Al-Cr refractories[J].Physical Testing and Chemical Analysis Part B: Chemical Analysis,2005,41(9):648-653.
[4]
金德龙,陆晓明,邰力.耐火材料X射线荧光光谱分析方法[J].耐火与石灰,2008,33(3):4-8.JIN De-long,LU Xiao-ming,TAI Li.The standard analysis method for determination refractory by XRFS[J].Refractories & Lime,2008,33(3):4-8.
[5]
吴增升,刘志民.X射线荧光光谱法分析镁砂中的主次成分[J].中国无机分析化学,2014,4(4):37-38.WU Zeng-sheng,LIU Zhi-min.Determination of major and minor components in magnesia by X-ray fluorescence spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2014,4(4):37-38.
[6]
陆晓明,邰力,金德龙.X射线荧光光谱法分析镁铬耐火材料[J].耐火材料,2006,40(3):231-233.LU Xiao-ming,TAI Li,JIN De-long.Determination of magnesia-chrome refracties by X-ray fluorescence spectrometry with fusion method[J].Naihuo Cailiao,2006,40(3):231-233.
[7]
陈新,胡晓静,欧阳昌俊,等.X射线荧光法对镁铬砂成分的定量测定[J].光谱实验室,2000,17(4):431-434.CHEN Xin,HU Xiao-jing,OUYANG Chang-jun,et al.Determination of major elements in chrome magnesite by XRF[J].Chinese Journal of Spectroscopy Laboratory,2000,17(4):431-434.
[8]
苗国玉,杜建民,董中华.镁砂的粉末直接压片法 X 荧光光谱分析[J].冶金分析,2001,21(1):53-55.MIAO Guo-yu,DU Jian-min,DONG Zhong-hua.X-ray fluorescence spectrometric analysis of magnesia powder pressed into disks[J].Metallurgical Analysis,2001,21(1):53-55.
[9]
李国会,徐国令,李晓莉.X射线荧光光谱法在耐火材料成分分析中的应用[J].岩矿测试,2003,22(3):217-220.LI Guo-hui,XU Guo-ling,LI Xiao-li.Application of X-ray fluorescence spectrometry in refractory material analysis[J].Rock and Mineral Analysis,2003,22(3):217-220.
[10]
王芙云,袁翠菊,任向阳.X射线荧光光谱法快速分析镁质耐火材料中硅铝铁钛钙镁[J].岩矿测试,2008,27(3):232-234.WANG Fu-yun,YUAN Cui-ju,REN Xiang-yang.Rapid determination of SiO2,Al2O3,Fe2O3,TiO2,CaO and MgO in magnesium-based refractory materials by X-ray fluorescence spectrometry with powder pellet sample preparation[J].Rock and Mineral Analysis,2008,27(3):232-234.
[11]
赵恩好,岳明新,周国兴,等.X射线荧光光谱法测定镁质耐火材料及其原料中10种成分[J].冶金分析,2013,33(7):62-67.ZHAO En-hao,YUE Ming-xin,ZHOU Guo-xing,et al.Determination of ten components in magnesia refractory materials and raw materials by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2013,33(7):62-67.
[12]
张鹏,曲月华,王一凌.X射线荧光光谱法测定镁砂、镁石及菱镁矿中主次成分[J].冶金分析,2010,30(9):28-31.ZHANG Peng,QU Yue-hua,WANG Yi-ling.Determination of major and minor elements in magnesia,humite and magnesite by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2010,30(9):28-31.
[13]
于杰,刘长春,丁健,等.镁质耐火材料-射线荧光光谱分析——粉末压片法与熔融玻璃片法之比较[J].辽东学院学报:自然科学版,2012,19(2):80-85.YU Jie,LIU Chang-chun,DING Jian,et al.Determination of magnesite refractory by XRF: a comparison of powder pressed method and glass flux sheet method[J].Journal of Eastern Liaoning University:Natural Science,2012,19(2):80-85.