Determination of Trace Organic Impurities in Refined TiCl4 by Infrared Spectroscopy

KeyWord:titanium tetrachloride  organic impurities  infrared spectroscopy  infrared liquid cell  quality control of titanium sponge

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£¨§¶25 mm¡Á2 mm,7 800-440 cm-1£© and a cell of PTFE£¨optical path£º10 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¡Á10-3,1.917¡Á10-3,1.554¡Á10-2,5.707¡Á10-3,3.769¡Á10-1 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.