一套红外池测定精四氯化钛中二氯氧钛的含量  

A Set of Infrared Cells for the Determination of Titanium Oxychloride in Refined Titanium Tetrachloride

作　　者：宋光林[1,2] 罗运军[1] 李晋庆[1] 李青 谭红 

机构地区：[1]北京理工大学材料学院,北京100081 [2]贵州省分析测试研究院,贵州贵阳550002

出　　处：《光谱学与光谱分析》2015年第12期3427-3430,共4页Spectroscopy and Spectral Analysis

基　　金：贵州省省长基金项目(黔省专合字[2012]19号);国家国际科技合作专项(2011DFB41640)资助

摘　　要：钛材质量控制的关键是控制精TiCl_4中杂质含量。精TiCl_4是海绵钛生产的关键环节,海绵钛中杂质与精TiCl4中杂质含量成4倍富集关系。需要分析氧杂质的来源,对精TiCl_4中氧杂质进行严格控制。精TiCl_4中TiOCl_2含量的测定具有重要意义。TiOCl2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(cx)与吸光度(A)~样品光程(L)曲线的斜率成正比,利用波长范围7 800~440cm^(-1)的硒化锌窗片(Φ10×1mm)和玻璃池体(22,12,7和4mm光程)组装成一套红外吸收池,采用加标法测定精TiCl_4中TiOCl_2杂质含量。实验得出TiOCl_2的检出限为17.8mg·kg^(-1),样品回归方程Y=1.0118 X,相关系数r为0.996 3,加标TiOCl_2样品的回归方程Y=1.940 0 X,相关系数r为0.997 0,线性关系较好。测定精TiCl4中TiOCl_2含量为833.8 mg·kg^(-1),标准偏差(SD)为40.0 mg·kg^(-1),方法精密度相对标准偏差(RSD)在0.95~1.94之间,加标回收率在88.5%~93.1%之间。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TiOCl_2含量,可满足精TiCl_4中TiOCl_2分析的要求。The content control of the impurities in refined TIC14 becomes the key part for the quality control of titanium material. Refined TiCh is the key procedure in producing titanium sponge. Besides, the content of the impurities in titanium sponge and that of the impurities in refined TICl4 presents the 4-times enrichment relationship. Therefore, control the content of the oxygen, there is the need to analyze the source of oxygen impurities so that strict control can be conducted over the impurities of refined TIC14. Determination of TiOCl2 in refined TICl4 was significant for analysis of its impurities. TiOC12 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 （Cr） and ahsorhance（A）-length （L） curve＇s slope have direct ratio. The infrared absorption cell with the window film of ZnSe （Ф× 1 mm, wavenumers; 7 800 -440 cm^-1 ） and the glass cell （optical path： 22, 12, 7 and 4 mm） was assembled and utilized in determination of the TiOCl2 in refined TIC14 by standard addition method. The detection limit of TiOCl2 was 17.8 mg · kg^-1 , the regression equation was Y= 1. 011 8X, R=0. 996 3; With standard addition method, the regression equation of TiOCI2 was Y= 1. 940 0X, R=0. 997 0, it＇ s good in linearity relation, the TiOC12 content in refined TiCI4 is determined to be 833.8 mg · kg^-1 and SD up to 40. 0 mg · kg^-1 RSD of the method precision is between 0. 95%-1. 94X, while recovery rate is between 88. 5-93.1%. 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 TiOCl2 content in refined TICl4 through adding standard sample for one time, it could meet the requi

关 键 词：红外池 测定 四氯化钛 二氯氧钛 

分 类 号：O657.3[理学—分析化学]