精四氯化钛中痕量有机杂质的红外光谱分析  

Determination of Trace Organic Impurities in Refined TiCl_4 by Infrared Spectroscopy

作　　者：谭红[1] 何锦林[1] 宋光林[1] 罗艳[1] 赵红波[1] 肖飞[1] 罗林[2] 郭鹏然[3] 李娜[3] 牟德海[3] 

机构地区：[1]贵州省理化测试分析研究中心,贵州贵阳550002 [2]贵州遵义钛厂,贵州遵义563000 [3]中国广州分析测试中心,广东广州510070

出　　处：《分析测试学报》2012年第10期1325-1329,共5页Journal of Instrumental Analysis

基　　金：科技部创新方法工作专项项目资助(2011IM030700)

摘　　要：精TiCl4中的CCl3COCl、CHCl2COCl、CH2ClCOCl、CS2和CCl4等痕量有机杂质具有明显差异的红外光谱特征,因而能够利用红外光谱实现同时测定。然而精TiCl4与空气中的水气接触后极易发生水解反应,生成强腐蚀性的盐酸烟雾,不能使用常规的红外液池进行测定。该文研究设计出波数范围为7 800～440 cm-1的硒化锌窗片(Ф25 mm×2 mm)和聚四氟乙烯池体(10 mm光程)组装式红外液池装置,采用标准加入法测定精TiCl4中的杂质含量。CCl3COCl、CHCl2COCl、CH2ClCOCl、CS2和CCl4的检出限分别为3.159×10-3、1.917×10-3、1.554×10-2、5.707×10-3、3.769×10-1mg·g-1。此组装红外液池装置具有安全、简便、易拆洗、不易损坏、可重复使用的特点,可满足海绵钛工业生产中精TiCl4的生产控制分析需要,具有良好的应用前景。The organic impurities in TiCI4, including CCI3COCI, CHCI=COC1, CH2C1COC1, CS2 and CC14, could be simultaneously determined by infrared spectral analysis due to the obvious differences of their infrared spectral characteristics. However, the traditional infrared liquid cell is not fit for the analysis of TiC14 sample, because TIC1, is easily hydrolyzed and could immediately reacts with moisture in the air to form highly corrosive hydrochloric acid smoke. In this paper, a new infrared measuring device with a window film of ZnSe （ Ф25 mm x 2 mm, 7 800 - 440 cm - l ） and a cell of PT- FE（ optical path： 10 mm） was assembled and used in determination of the five organic impurities by the standard addition method. The detection limits of CC13COC1, CHC12COC1, CH=C1COC1, CS2 and CC14 were,3. 159 x 10^-3, 1.917 x 10^-3, 1.554 X 10^-2, 5.707 x 10^-3, 3.769 x 10-1 mg . g-1 , respectively. The new infrared measuring device was safe, simple, easily removable, washable and reuseable, and the new method has a good application prospect in the real sample analysis and quality control of refined TiC14 in titanium sponge.

关 键 词：四氯化钛 有机杂质 红外光谱 红外液池 海绵钛质量控制 

分 类 号：O657.3[理学—分析化学] O614.411[理学—化学]