Abstract：The content of titanium is an indicator of ferrosilicon,so the accurate and rapid determination of titanium is very important.The sample was dissolved with nitric acid-hydrofluoric acid-perchloric acid system in experiments. Silicon was removed by volatilization through perchloric acid smoke.Moreover,the influence of matrix effect was eliminated using matrix matching method during the preparation of standard titanium solution series.Ti 334.94 nm was selected as the analysis line.The content of trace titanium in ferrosilicon was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES).The results of interference experiments of coexisting elements showed that calcium and manganese had no influence on the determination of titanium.Under the optimized working parameters, the linear correlation coefficient (r) of calibration curve for titanium was 0.999 8.The limit of detection and the limit of quantification of this method was 0.000 54% (mass fraction,same as below) and 0.001 8%, respectively.The experimental methods were used to determine trace titanium in certified reference materials and actual samples of ferrosilicon.The relative standard deviations (RSD, n=11) of the measured results were between 1.8% and 2.7%.The measured value of certified reference materials (YSB14614-2008 and YSBC28605a-2013) were consistent with the certified value. The spiked recoveries of titanium in ferrosilicon sample (wTi=0.005 7%) were between 99% and 104%.
[1] 侯列奇,李洁,王树安,等.电感耦合等离子体原子发射光谱法测定硅铁材料中10种微量元素[J].冶金分析, 2008,28(1):52-54. HOU Lieqi,LI Jie,WANG Shu′an,et al.Determination of ten trace elements in ferrosilicon materials by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2008,28(1):52-54. [2] 霍红英,张勇.稀土硅铁合金中钛含量测定[J].化工进展,2014,33(1):183-186. HUO Hongying,ZHANG Yong.Determination of titanium content in rare earth ferrosilicon alloy[J].Chemical Industry and Engineering Progress,2014,33(1):183-186. [3] 张遴.钛铁试剂光度法测定硅铁中钛[J].理化检验(化学分册),2003,39(6):363-364. ZHANG Lin.Determination of titanium in ferrosilicon by spectrophotometric method with ferro-titanium reagent[J]. Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2003,39(6):363-364. [4] 李玉梅,杜梅,郝茜,等. ICP-AES法测定稀土硅铁及镁硅铁合金中钛的含量[J].稀土,2014,35(1):92-95. LI Yumei,DU Mei,HAO Qian,et al.Determination of titanium content in rare earth ferrosilicon and magnesium ferrosilicon alloy by ICP-AES[J].Chinese Rare Earth,2014,35(1):92-95. [5] 孙丽丽.电感耦合等离子体发射光谱仪测定磷酸中铅、砷、镉、铬[J].磷肥和复肥,2012,27(3):65. SUN Lili.Determination of lead, arsenic, cadmium and chromium in phosphoric acid by inductively coupled plasma spectroscopy[J].Phosphate & Compound Fertilizer,2012,27(3):65. [6] 董礼男,周莉莉,赵希文,等.微波消解-电感耦合等离子体原子发射光谱法测定甲基磺酸盐(MSA)电镀锡泥中铜镍铅锑铋[J].冶金分析,2021,41(7):47-53. DONG Linan,ZHOU Lili,ZHAO Xiwen,et al.Determination of copper, nickel, lead, antimony and bismuth in methanesulfonate (MSA) electroplating tin mud by microwave digestion-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2021,41(7):47-53. [7] 成勇,刘力维,袁金红,等.电感耦合等离子体原子发射光谱法测定熔盐废渣中钪和钛[J].冶金分析,2021, 41(7):75-81. CHENG Yong,LIU Liwei,YUAN Jinhong,et al.Determination of scandium and titanium in molten salt waste residue by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2021,41(7):75-81. [8] 周元敬,龙尚俊,李家华,等.电感耦合等离子体原子发射光谱法测定铝合金中镧、铈、钪的含量[J].理化检验(化学分册),2017,53(12):1427-1431. ZHOU Yuanjing,LONG Shangjun,LI Jiahua,et al.Determination of the content of lanthanum,cerium and sca-ndium in aluminum alloy by inductively coupled plasma atomic emission spectrometry[J].Physical Testing and Chemical Analysis(PartB:Chemical Analysis),2017,53(12):1427-1431. [9] 宋祖峰,陆向东,荚江霞,等.电感耦合等离子体原子发射光谱法测定低碳低钛硅铁中痕量铌钒锆[J].冶金分析,2018,38(5):35-40. SONG Zufeng,LU Xiangdong,JIA Jiangxia,et al.Determination of trace niobium,vanadium and zirconium in low carbon and low titanium ferrosilicon by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(5):35-40.
