Determination of titanium dioxide in limestone and dolomite by spectrophotometry
DENG Junhua1,2, KANG Dehua1,2
1. State Key Laboratory of Metal Material for Marine Equipment and Application,Anshan 114009, China; 2. Iron & Steel Research Institute of Ansteel Group, Liaoning, Anshan 114009, China
Abstract：In recent years, the content of titanium in pure steel and cord steel is strictly controlled. Therefore, the whole process monitoring requirements have been put forward for the titanium dioxide content in metallurgical materials. Limestone and dolomite are widely used as important metallurgical raw materials in the iron and steel industry. Since there is no national standard method for the determination of titanium dioxide content in limestone, the establishment of a method for the accurate determination of titanium dioxide content in limestone and dolomite is of great significance. In experiments, the content of titanium dioxide in limestone and dolomite was determined by diantipyrine methane spectrophotometry. The sample was melted at high temperature using boric acid and sodium carbonate mixture as the flux. Based on the character that diantipyrine methane could react with Ti (IV) to form a stable yellow complex (1∶3) [Ti (DAPM)3]4+, the content of titanium dioxide was determined by spectrophotometry. Under the optimized experimental conditions, Bill's law was obeyed for titanium dioxide with mass fraction in range of 0-1.40 mg/L. At wavelength of 385 nm, the apparent molar absorptivity was 1.39×104 L·mol-1·cm-1. The linear correlation coefficient of the calibration curve was 0.999. The proposed method was applied for the determination of certified reference materials including GBWQD10-119, YSBC28709a-2013, YSBC28713a-2013 and SX07-10. The found results were consistent with the certified values. The relative standard deviations (RSD, n=6) of determination results were between 1.6% and 2.6%. The precision tests were conducted by nine steel industry laboratories accredited by China National Accreditation Service for Conformity Assessment (CNAS) in China, and it was proved that the proposed method had good repeatability and reproducibility. The content of titanium dioxide (0.005 0%-0.30%) in limestone and dolomite was determined according to the experimental method. The regression equation of repeatability limit (r) was lgr=0.801 0 lgm-1.468 3, the regression equation of reproducibility (R) was lgR=0.849 2 lgm-1.189 7.
邓军华, 亢德华. 分光光度法测定石灰石及白云石中二氧化钛[J]. 冶金分析, 2022, 42(2): 58-63.
DENG Junhua, KANG Dehua. Determination of titanium dioxide in limestone and dolomite by spectrophotometry. , 2022, 42(2): 58-63.
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