Calibration curve and mass correction in fuse beadsanalysis of X-ray fluorescence spectrometry
XU Jian-ping1, ZHANG Zhao-xiong2
1. The National Key Lab of Refractory Material and Metallurgy,Wuhan University of Science and Technology,Wuhan 430081, China; 2. The Quality Inspection Center of Wuhan Iron and Steel Co., Ltd., Wuhan 430080, China
Abstract：In fuse beads analysis of iron alloy and iron ore by X-ray fluorescence spectrometry, there was some error caused by the sample mass difference between direct ignition and fusion, and it could not be corrected by the conventional dilution ratio correction method. A series of tested oxide components were added into flux of fixed mass (volume) to prepare glass beads standard series with same mass (volume). The function curve was established between X-ray fluorescence intensity and volume concentration of tested component in glass beads. The analytical results were calibrated with the mass ratio of sample glass beads to that of calibration curve. In other words, the dilution ratio correction was replaced by mass correction. With pure substances (SiO2, CaCO3, Al2O3 and Fe2O3) as standards, the calibration curve between the mass fraction and fluorescence intensity of Si, Ca, Fe and Al was established for analysis of calcium-silicon alloy under the selected instrumental working conditions. The linear correlation coefficient was 0.9990, 0.9993, 0.9994 and 0.9995, respectively. The accuracy of calibration curve was verified with the certified reference material. The t test results showed that when the mass change of glass beads was large, the determination results without mass correction had great deviation with low accuracy.
Terrance Hettipathirana,Naomi Grey,Ravi Naidu.Elimination of analytical error due to the use of catch weights with loss-eliminated alphas in X-ray fluorescence spectrometric analysis of limestone using borate fusions[J].Spectrochimica Acta Part B,2003,58:85-95.
[2]
张建波,王谦,林力,等.锰的价态研究及在X射线荧光光谱测定锰矿中的应用[J].冶金分析,2011,31(4):20-25.ZHANG Jian-bo,WANG Qian,LIN Li,et al.Study on chemical valence of manganese and its application in X-ray fluorescence spectrometry determination of manganese ore[J].Metallurgical Analysis,2011,31(4):20-25.
[3]
梁国立,邓赛文,刘以建.X射线荧光分析中熔融制样的稀释率和烧失量校正[J].岩矿测试,1995,14(3):189-192.LIANG Guo-li,DENG Sai-wen,LIU Yi-jian.Correction for dilution ratio and loss on ignition in the application of fusion beads method in XRF sample preparation[J].Rock and Mineral Analysis,1995,14(3):189-192.
[4]
韩蔚,梅一飞,周建.荧光熔剂熔融损失对XRF分析的影响[J].中国建材科技,2015(1):1-3.HAN Wei,MEI Yi-fei, ZHOU Jian.The influence of fluorescence flux meltin gloss to XRF analysis[J].Chinese Building Materials Science & Technology,2015(1):1-3.
[5]
童晓民,赵宏风,张伟民.熔片X射线荧光光谱法测定矿物中钨和钼[J].冶金分析,2007,27(5):25-28.TONG Xiao-min,ZHAO Hong-feng,ZHANG Wei-min.Determination of tungsten and molybdenum in materials by fusion beads X-ray fluorescence spectrometry[J].Metallurgical Analysis,2007,27(5):25-28.
[6]
彭慧仙.熔融制样-X射线荧光光谱法测定硬质合金中钨钴镍铁铌钽铬[J].冶金分析,2015,35(7):20-26.PENG Hui-xian.Determination of tungsten,coalt,nickel,iron,niobium,tantalum and chromium in hard alloy by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2015,35(7):20-26.
[7]
徐建平.四硼酸锂坩埚内预氧化熔融制样-X射线荧光光谱法测定锰铁及锰硅合金中的硅、锰、磷[J].理化检验:化学分册(Pyhsical Testing and Chemical Analysis Part B:Chemical Analysis),2016,52(11):1344-1346.
Rosalind R Schwarz,David McCallum.Analysis of ferrosilicon and silicon carbide by an X-ray fluorescence fusion method-an X-ray diffraction investigation of the preliminary oxidation[J].Analytical Communications,1997,34(6):165-169.
[10]
鲍希波,石毓霞,赵靖,等.熔融制样-X射线荧光光谱法测定硅铁合金中主次元素[J].冶金分析,2010,30(5):14-18.BAO Xi-bo,SHI Yu-xia,ZHAO Jing,et al.X-ray fluorescence spectrometry for the determination of major and minor elements in ferro-silicon alloy with fusion sample preparation[J].Metallurgical Analysis,2010,30(5):14-18.
[11]
王平英,陈鹏飞.熔融制样-X射线荧光光谱法测定高碳铬铁中铬、硅和磷的含量[J].理化检验:化学分册,2014,50(8):1024-1026.WANG Ping-ying,CHEN Peng-fei.Determination of chromium,silicon and phosphorus in high carbon ferrochrome by X-ray fluorescence spectrometry[J].Pyhsical Testing and Chemical Analysis Part B:Chemical Analysis,2014,50(8):1024-1026.
[12]
杨觎,边立槐,孙颖.熔融制样-X射线荧光光谱法测定铌铁合金中的铌铝钛[J].天津冶金,2009(4):54-55.YANG Yu,BIAN Li-huai,SUN Ying.Determination of Nb-Al-Ti in ferrocolumbium by X-ray fluorescence spectrometry with fusion sample preparation[J].Tianjin Metallurgy,2009(4):54-55.
[13]
廖海平,付冉冉,张建波,等.熔融制样-X射线荧光光谱法测定直接还原铁中主次元素含量[J].理化检验:化学分册,2014,50(1):31-34.LIAO Hai-ping,FU Ran-ran,ZHANG Jian-bo,et al.XRFS determination of major and minor elements in direct reduction-iron with sample preparation by fusion[J].Pyhsical Testing and Chemical Analysis Part B:Chemical Analysis,2014,50(1):31-34.
[14]
陈美芳,黄光明,江冶,等.X射线荧光光谱分析在我国铁矿石分析中的应用[J].地质学刊,2012,36(2):206-211.CHEN Mei-fang,HUANG Guang-ming,JIANG Ye,et al.Application of X-ray fluorescence in analysis of iron ore in China[J].Geological Journal,2012,36(2):206-211.
[15]
李韶梅.X射线荧光光谱法测定复合碳铁合金中总铁含量[J].冶金分析,2012,32(4):54-56.LI Shao-mei.Determination of total iron in carbon iron by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2012,32(4):54-56.
