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精TiCl_4是海绵钛生产的关键环节,且海绵钛中杂质碳和氧(C,O)与精TiCl_4中杂质C和O含量成4倍富集关系,因此,钛材质量控制的关键是控制精TiCl_4中杂质C和O的含量。为了控制精TiCl_4中的C和O,需要分析C和O杂质的来源,对精TiCl_4中杂质进行严格控制。测定精TiCl_4中CO2的含量,对精TiCl_4中杂质C和O的分析具有重要意义。CO_2具有红外吸收谱线,因而能够利用红外光谱实现测定,然而精TiCl_4与空气中水气接触极易发生水解反应,生成强腐蚀性的盐酸烟雾,不能使用常规的红外吸收池进行测定。根据Lambert-Beer定律,被测组分浓度(c_x)与吸光度(A)~样品光程(L)曲线的斜率成正比,本研究利用波数范围7 800~440 cm~(-1)的硒化锌窗片(φ10 mm×1 mm)和玻璃池体(42,22,12,7和4 mm光程)组装成一套红外吸收池,采用加标法测定精TiCl_4中CO_2杂质含量。实验得出CO_2的检出限为0.92 mg·kg~(-1),样品回归方程Y=0.031 1X,相关系数r为0.997 2,加标CO_2样品的回归方程Y=0.131 7X,相关系数r为0.998 6,线性关系较好,测定精TiCl_4中CO_2含量为1.53 mg·kg~(-1),标准偏差(SD)为0.04 mg·kg~(-1),方法相对标准偏差(RSD)在0.53%~1.27%之间,加标回收率在89.2%~96.8%。此红外吸收池安全简便、容易拆洗、可重复使用,通过一次加标样品定量分析精TiCl_4中CO_2含量,可满足精TiCl_4中CO_2分析的要求。
Fine TiCl_4 is a key step in the production of titanium sponge. The content of carbon and oxygen (C, O) in the sponge titanium and the impurities C and O in the refined TiCl_4 are four times enrichment. Therefore, the key of titanium quality control is to control fine The content of impurities C and O in TiCl_4. In order to control the C and O in the refined TiCl 4, the source of the C and O impurities needs to be analyzed, and the impurities in the refined TiCl 4 are strictly controlled. The determination of CO2 content in refined TiCl4 is of great significance for the analysis of impurities C and O in refined TiCl4. CO_2 with infrared absorption spectrum, which can be measured using infrared spectroscopy, however, fine TiCl_4 contact with water vapor in the air prone to hydrolysis reaction, the formation of highly corrosive hydrochloric acid smoke can not be measured using a conventional infrared absorption cell. According to Lambert-Beer’s law, the concentration of the measured component (cx) is proportional to the slope of the absorbance (A) to the optical path of the sample (L) curve. In this study, selenium with a wavenumber range of 7 800 to 440 cm -1 Zinc window (φ10 mm × 1 mm) and glass cell body (42, 22, 12, 7 and 4 mm pathlength) were assembled into a set of infrared absorption cell. The content of CO 2 in refined TiCl 4 was determined by spike method. The detection limit of CO_2 was 0.92 mg · kg -1, the regression equation of the sample was Y = 0.031 1X, the correlation coefficient was 0.997 2, the regression equation of spiked CO_2 was Y = 0.131 7X, the correlation coefficient r was 0.998 6. The linear relationship was good. The CO 2 content in refined TiCl 4 was 1.53 mg · kg -1, the standard deviation (SD) was 0.04 mg · kg -1, and the relative standard deviation (RSD) was 0.53 % ~ 1.27%, the spiked recoveries ranged from 89.2% to 96.8%. The infrared absorption cell is safe, easy to disassemble and wash, and can be reused. The CO 2 content in refined TiCl 4 can be quantitatively analyzed by a spiked sample to meet the requirements of CO 2 analysis in refined TiCl 4.