【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。更多还原

【Abstract】 The organic impurities in TiCl4,including CCl3COCl,CHCl2COCl,CH2ClCOCl,CS2 and CCl4,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 TiCl4 sample,because TiCl4 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×2 mm,7 800-440 cm-1) and a cell of PTFE(optical path:10 mm) was assembled and used in determination of the five organic impurities by the standard addition method.The detection limits of CCl3COCl,CHCl2COCl,CH2ClCOCl,CS2 and CCl4 were 3.159×10-3,1.917×10-3,1.554×10-2,5.707×10-3,3.769×10-1 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 TiCl4 in titanium sponge.更多还原