Determination of titanium, phosphorus, silicon, manganese and aluminum in ferrotitanium by X-ray fluorescence spectrometry with fusion sample preparation
QI Wei, GAO Yanqiang, SONG Miao, WANG Xiaoxia, LIU Yanhui
Ningbo Iron and Steel Co., Ltd.,Ningbo 315807,China
Abstract：During the determination of major and minor elements in ferrotitanium by the traditional chemical wet analysis method, the operation was time-consuming and difficult to master. The application of X-ray fluorescence spectrometry(XRF) for determination of ferrotitanium was explored. The sample was dissolved with sulfuric acid (1+10). The pre-oxidation technology of low temperature heating evaporation, fuming sulfuric acid and high temperature heating were adopted to solve the problem that the platinum-gold crucible was easily damaged due to the formation of low temperature eutectic between alloying element and platinum during high-temperature fusion of ferrotitanium alloy. The effects of concentration and dosage of sulfuric acid, sample dissolution conditions, dilution ratio, fusion temperature and fusion time on the determnaiton results were investigated. The optimal conditions were obtained as follows: 10 mL of sulfuric acid (1+10) was used to dissolve the sample; the solution was heated to exhaust sulfuric acid smoke; the dilution ratio was 1∶40; the fusion temperature and time was 1 100 ℃ and 15 min, respectively. Consequently, the calibration curves for determination of titanium, phosphorus, silicon, manganese, and aluminum in ferrotitanium by X-ray fluorescence spectrometry with fusion sample preparation were established. The correlation coefficients of calibration curves were all greater than 0.993. The ferrotitanium sample was selected to prepared twelve parallel glass sheet for precision test. The relative standard deviations (RSD, n=12) of the determination results for five elements were between 0.15% and 5.0%. The proposed method was applied to determination of titanium, phosphorus, silicon, manganese, and aluminum in ferrotitanium certified reference materials. The results were consistent with the certified values. For ferrotitanium samples, the determination results of the proposed method were consistent with those obtained by national or industry standard methods. The proposed method could meet the daily testing requirements of ferrotitanium alloy.
[1] 王静静. X-射线荧光光谱仪测定钛铁中Si、Mn、P、Al、Cu[J].河北化工(Hebei Chemical Industy),2012(1):65-66. [2] 杨平,金爱娣.X荧光光谱法测定钛铁中Ti、Si、P、Mn、Cu[C]//第17届全国铁合金学术研讨会论文集.桂林:中国金属学会铁合金分会,2008:217-219. [3] 常利民,刘峰,王晓霞,等.基于熔融制样测量钛铁中5种成份的研究[J].中国测试(China Measurement & Test),2017,43(增1):68-71. [4] 邢文青,马秀艳,曾赞喜,等.熔融法制样-X射线荧光光谱法测定钛铁中5种元素含量[J].理化检验(化学分册)(Physical Testing and Chemical Analysis(Part B:Chemical Analysis)),2018,54(3):312-316. [5] Claisse F,Samson C.Heterogeneity effects in X-ray analysis[J].Advances in X-ray Analysis,1962(5):335-354. [6] 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 Xibo,SHI Yuxia,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. [7] 刘伟,曹吉祥,郭云涛,等.熔融制样-X射线荧光光谱法测定硅锰合金中的硅锰磷[J].冶金分析,2015,35(8):51-54. LIU Wei,CAO Jixiang,GUO Yuntao,et al.Determination of silicon,manganese,phosphorus in silicon-manganese alloy by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2015,35(8):51-54. [8] 李国会,李小莉.X射线荧光光谱分析熔融法制样的系统研究[J].冶金分析,2015,35(7):1-9. LI Guohui,LI Xiaoli.Systematic study on the fusion sample preparation in X-ray fluorescence spectrometry analysis[J].Metallurgical Analysis,2015,35(7):1-9. [9] 宫嘉辰,白小叶,姜炳南.熔融制样-X射线荧光光谱法测定钒钛磁铁矿中12种组分[J].冶金分析,2019,39(2):66-70. GONG Jiachen,BAI Xiaoye,JIANG Bingnan.Determination of twelve components in vanadium-titanium magnetite ore by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2019,39(2):66-70. [10] 郑晓敏,於利慧.熔融制样-X射线荧光光谱法测定酸溶性钛渣中主次量成分[J].冶金分析,2019,39(11):16-23. ZHENG Xiaomin,YU Lihui.Determination of major and minor components in acid-soluble titanium slag by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2019,39(11):16-23. [11] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 4701.2—2009 钛铁 硅含量的测定 硫酸脱水重量法[S].北京:中国标准出版社,2009. [12] 中华人民共和国国家质量监督检验检疫总局.SN/T 3367—2012钛铁中钛、铝、硅、磷、铜、锰含量的测定 电感耦合等离子体原子发射光谱法[S].北京:中国标准出版社,2012. [13] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 4701.6—2009 钛铁 铝含量的测定 EDTA滴定法[S].北京:中国标准出版社,2009. [14] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 4701.7—2009 钛铁 磷含量的测定 铋磷钼蓝分光光度法和钼蓝分光光度法[S].北京:中国标准出版社,2009. [15] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 4701.1—2009 钛铁 钛含量的测定 硫酸铁铵滴定法[S].北京:中国标准出版社,2009.
