Determination of total oil in refined titanium tetrachloride by hydrolysis-infrared absorption spectroscopy
WANG Yanjiao1, ZOU Xiaonan2, ZU Yue3, SONG Guanglin*1
1. Guizhou Academy of Analysis and Testing,Guiyang 550016,China; 2. Guizhou Engineering Vocational College Scientific Bureau,Tongren 565200,China; 3. Guizhou Testing Technology Reserch and Application Center,Guiyang 550016,China
Abstract：The refined titanium tetrachloride is the key raw material to produce sponge titanium and titanium. The key to improve the quality of sponge titanium and titanium is to control the impurity content in refined titanium tetrachloride. Due to the production process, the carbon impurities in refined titanium tetrachloride are mainly oil impurities, so the determination of oil impurities in refined titanium tetrachloride is of great significance to the analysis of carbon impurities in refined titanium tetrachloride. The total oil is mainly composed of carbon which has infrared absorption band, so it can be determined by infrared absorption spectroscopy. However, titanium tetrachloride is easily hydrolyzed when contacting with water and air, and the generated hydrogen chloride also has infrared absorption peak. Moreover, the wave number of absorption peaks of hydrogen chloride and oils is close. As a result, hydrogen chloride interferes with the determination of total oil content in the original titanium tetrachloride sample by infrared absorption spectroscopy.A method for the determination of total oil content in refined titanium tetrachloride by hydrolysis-infrared absorption spectroscopy was established. The titanium tetrachloride sample was hydrolyzed using water with a volume ratio of 1∶25. After equilibrium, the total oil in the hydrolyzed solution was extracted by tetrachloroethylene. The content of total oil in refined titanium tetrachloride was quantitatively analyzed by external standard method. The linear range of total oil in calibration curve was 0-80 mg/L with correlation coefficient (r) of 0.999 9. The limit of detection of total oil was 2.5 mg/kg. The proposed method was applied for the determination of total oil in refined titanium tetrachloride sample. The relative standard deviations (RSD, n=6) of determination results were between 3.5% and 4.1%, and the spiked recoveries were between 96% and 109%.
王艳娇, 邹小南, 祖跃, 宋光林. 水解-红外吸收光谱法测定精四氯化钛中总油[J]. 冶金分析, 2022, 42(8): 76-80.
WANG Yanjiao, ZOU Xiaonan, ZU Yue, SONG Guanglin. Determination of total oil in refined titanium tetrachloride by hydrolysis-infrared absorption spectroscopy. , 2022, 42(8): 76-80.
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