Abstract:The contents of TiO2, SiO2, CaO, MnO, MgO and TFe in high titanium slag are usually determined by titrimetric methods or photometric methods. However, these methods are relatively time-consuming, the consumption of chemical reagents is large, and the workload is heavy. Therefore, it is necessary to develop a simple and rapid analysis method with high accuracy for the simultaneous determination of multi-elements. The sample was prepared by powder pressing method. The six components including TiO2, SiO2, CaO, MnO, MgO and TFe in high titanium slag were determined by energy dispersive X-ray fluorescence spectrometry (EDXRF). High titanium slag with particle size of 20 μm was selected, and boric acid was used as binder to edge the bottom. The samples prepared under the experimental conditions (pressure of 25 MPa and holding time of 5 min) were smooth and crack-free, and could be stored for a long time. Due to the shortage of high titanium slag standard sample, according to the content range of each component in the high titanium slag sample, the calibration curve was established using self-made reference standard samples with certain concentration gradient, which were prepared by certified reference materials of high titanium slag and high-purity reagents. Meanwhile, the matrix effect was corrected by fundamental parameter method. The correlation coefficients of calibration curves for testing components were not less than 0.998 0. The limits of detection (LOD) were between 0.002 5% and 0.037%. The relative standard deviations (RSD, n=8) of determination results were between 0.10% and 1.5%. The proposed method was applied for the analysis of actual high titanium slag samples, and the found results were in good agreement with those obtained by chemical wet method in industrial standard YS/T 514 series.
谢秀琼, 霍红英. 粉末压片-能量色散X射线荧光光谱法测定高钛渣中6种组分[J]. 冶金分析, 2021, 41(2): 34-39.
XIE Xiuqiong, HUO Hongying. Determination of six components in high titanium slag by energy dispersive X-ray fluorescence spectrometry with pressed powder pellet. , 2021, 41(2): 34-39.
逯冉,贾翃.我国高钛渣生产技术现状及发展分析[J].中国金属通报,2014(10):43-45.LU Ran,JIA Hong.Present situation and development analysis of production technology of high titanium slag in China[J].China Metal Bulletin,2014(10):43-45.
[2]
黄世弘.直流密闭电炉冶炼高钛渣的元素分配及生产工艺技术研究[D].昆明:昆明理工大学,2016.
[3]
刘洪涛,邵常丽.能量色散X射线荧光光谱法测定铁矿石中化学成分[J].冶金分析,2016,36(6):69-72.LIU Hongtao,SHAO Changli.Determination of chemical components in iron ores by energy dispersive X-ray fluorescence spectrometry[J].Metallurgical Analysis,2016,36(6):69-72.
[4]
罗明荣,陈文静.X射线荧光光谱法测定还原钛铁矿中11种组分[J].冶金分析, 2012,32(6):24-29.LUO Mingrong,CHEN Wenjing.X-ray fluorescence spectrometric determination of eleven components in reduced ilmenite[J].Metallurgical Analysis,2012,32(6):24-29.
[5]
胡波,武晓梅,余韬,等. X射线荧光光谱仪的发展及应用[J].核电子学与探测技术,2015,35(7):695-702,706.HU Bo,WU Xiaomei,YU Tao,et al.The development and application of X-ray fluorescence spectrometer[J].Nuclear Electronics and Detection Technology,2015,35(7):695-702,706.
[6]
Orlic M,Badovinac I J.Evaluation of elemental concentrations in environmental specimens using X-ray fluorescence and micro-raman spectroscopy[J].Nuclear Instruments and Methods in Physics Research,2013,19(5):86-88.
[7]
Sun T,Ding X L.Determination of the properties of a polycapillary X-ray spectrometry[J].X-Ray Spectrometry, 2014,35(46):120-252.
[8]
刘江斌,党亮,殷桃刚.粉末压片-X射线荧光光谱分析中区域地球化学样品制备和标准曲线建立的几点认识[J].甘肃地质,2015,24(4):84-87.LIU Jiangbin,DANG Liang,YIN Taogang.Geochemical sample preparation and establishment of standard curve for X-ray fluorescence spectrometry analysts with pressed powder pellet[J].Gansu Geology,2015,24(4):84-87.
[9]
刘尚华,陶光仪,吉昂.X射线荧光光谱分析中粉末压片制样法[J].光谱实验室,1988(6):10-16.LIU Shanghua,TAO Guangyi,JI Ang.Powder tablet sampling method in X-ray fluorescence spectrometry analysis[J].Chinese Journal of Spectroscopy Laboratory,1998(6):10-16.
[10]
武映梅,石仕平,宋武元.X射线荧光光谱粉末压片法检测合金铸铁中13种成分[J].冶金分析,2012,32(7):32-37.WU Yingmei,SHI Shiping,SONG Wuyuan.Determination of thirteen components in cast iron by X-ray fluorescence spectrometry with power press method[J].Metallurgical Analysis,2012,32(7):32-37.
[11]
豆卫全,高明,夏培民,等.粉末压片-能量色散X射线荧光光谱法分析硅铬合金中铬硅磷[J].冶金分析,2019,39(9):54-58.DOU Weiquan,GAO ming,XIA Peimin,et al.Determination of chromium,silicon and phosphorus in silicochrome by energy dispersive X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis,2019,39(9):54-58.
[12]
曾江萍,张莉娟,李小莉,等.超细粉末压片-X射线荧光光谱法测定磷矿石中12种组分[J].冶金分析,2015,35(7):37-43.ZENG Jiangping,ZHANG Lijuan, LI Xiaoli,et al.Determination of 12 components in phosphorus ore by ultrafine powder tablet-X-ray fluorescence spectrometry[J].Metallurgical Analysis,2015,35(7):37-43.
[13]
赵合琴,郑先君,魏丽芳,等.X射线荧光光谱分析中样品制备方法评述[J].河南化工,2006(10):8-11.ZHAO Heqin,ZHENG Xianjun,WEI Lifang.Review of sample preparation methods in X-ray fluorescence spectrometry[J]. Henan Chemical Industry,2006(10):8-11.
[14]
单华珍,卓尚军,盛成,等.粉末压片法波长色散 X射线荧光光谱分析铁矿石样品的矿物效应校正初探[J].光谱学与光谱分析,2008(7):1661-1664.SHAN Huazhen,ZHUO Shangjun,SHENG Cheng,et al.Preliminary study on mineral effect correction of iron ore samples by wavelength dispersion X-ray fluorescence spectrometry by powder pressing method[J].Spectroscopy and Spectral Analysis,2008(7):1661-1664.
[15]
徐建平,程德翔.包覆效应与压片法X射线荧光光谱分析[J].理化检验(化学分册),2015,51(2):219-223.XU Jianping,CHENG Dexiang.Coating effect in XRFS analysis with pressing discs[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis),2015,51(2):219-223.