光谱学与光谱分析, 2015, 35 (3): 626, 网络出版: 2015-05-21   

红外光谱法测定精四氯化钛中二氧化碳的含量

Determination of Carbon Dioxide in Refined Titanium Tetrachloride by Infrared Spectroscopy
作者单位
1 北京理工大学材料科学与工程学院, 北京 100081
2 贵州省分析测试研究院, 贵州 贵阳 550002
摘要
精TiCl4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TiCl4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TiCl4中杂质C和O的含量。 为了控制精TiCl4中的C和O, 需要分析C和O杂质的来源, 对精TiCl4中杂质进行严格控制。 测定精TiCl4中CO2的含量, 对精TiCl4中杂质C和O的分析具有重要意义。 CO2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TiCl4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(cx)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(10 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TiCl4中CO2杂质含量。 实验得出CO2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CO2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TiCl4中CO2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TiCl4中CO2含量, 可满足精TiCl4中CO2分析的要求。
Abstract
Refined TiCl4 is the key procedure in producing titanium sponge. Besides, the content of carbon and oxygen (C and O) impurities in titanium sponge and that of C and O impurities in refined TiCl4 presents the 4-times enrichment relationship. Therefore, the content control of the C and O impurities in refined TiCl4 becomes the key part for the quality control of titanium material. In order to control the oxygen and carbon, there is the need to analyze the source of C and O impurities so that strict control can be conducted over the impurities of refined TiCl4. Determination of CO2 in refined TiCl4 was significant for analysis of its impurities. CO2 could be determined by infrared spectroscopy due to its infrared characteristic spectrum line. However, normal infrared absorption cell was not fit for the sample analysis, because TiCl4 easily reacted with moisture in the air and immediately was hydrolyzed to form highly corrosive hydrochloric acid smoke. According to Lambert-Beer Law, which means the concentration (cx) and absorbance(A)~length (L) curve’s slope have direct ratio. The infrared absorption cell with the window film of ZnSe ( 10 mm×1 mm, wavenumers: 7 800~440 cm-1) and the glass cell (optical path: 42, 22, 12, 7 and 4 mm) was assembled and utilized in determination of the CO2 in refined TiCl4 by standard addition method. The detection limit of CO2 was 0.92 mg·kg-1, the regression equation was Y=0.031 1X, R=0.997 2; With standard addition method, the regression equation of CO2 was Y=0.131 7X, R=0.998 6, it’s good in linearity relation, the CO2 content in refined TiCl4 is determined to be 1.53 mg·kg-1 and SD up to 0.04 mg·kg-1. RSD of the method precision is between 0.53%~1.27%, while recovery rate is between 89.2%~96.8%. This infrared absorption device was safe, simple and convenient, easily removable and washable, and re-useable. The method could conduct the quantitative analysis over the CO2 content in refined TiCl4 through adding standard sample for one time, it could meet the requirement of determination of CO2 in refined TiCl4.

宋光林, 罗运军, 李晋庆, 谭红. 红外光谱法测定精四氯化钛中二氧化碳的含量[J]. 光谱学与光谱分析, 2015, 35(3): 626. SONG Guang-lin, LUO Yun-jun, LI Jin-qing, TAN Hong. Determination of Carbon Dioxide in Refined Titanium Tetrachloride by Infrared Spectroscopy[J]. Spectroscopy and Spectral Analysis, 2015, 35(3): 626.

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