红外光谱法分析生产中回收高纯SiCl4中有机杂质

探索了遵义钛厂海绵钛生产中回收高纯四氯化硅新工艺中有机杂质的红外色谱分析方法.针对四氯化硅极易水解的特点,设计了一套密封取样装置,自制密封红外玻璃样品池,采用FT-IR FTS4000红外光谱仪,在4000～1000 cm~(-1)波段内对高纯四氯化硅样品测量得到红外光谱,通过与美国Merck公司标准品四氯化硅(99.9999%)红外光谱图对比,发现在2257 cm~(-1)未出现吸收带,可断定样品中不含有三氯氢硅.针对光谱图中3700～3500 cm~(-1)之间-OH的吸收带,选用与四氯化硅极性相似的化学物质CCl_4做基体溶液,用三苯基硅醇标准加入法实现了-OH基团的定量分析,相关系数r为0.9963,摩尔吸光系数ε=108 L·mol~(-1)·cm~(-1).

Study on infrared spectrophotometric determination of the organic impurity of SiCl4 recycled from the sponge titanium process

Preliminary study on infrared spectrophotometric determination of the organic impurity of high purity SiCl_4 recycled from the sponge titanium process.SiCl_4 is easy to hydrolyze when it is exposed in air,therefore,a sealing unit was designed to get the samples,including a sealing infrared sample cell which was made by ourself.The high purity SiCl_4 was analyzed at the wave band of 4000～1000 cm~(-1) by FT-IR FTS4000 infrared spectrometer.Infrared spectrum showed that the absorption peak of SiHCl_3 at 2257 cm~(-1) was not exsited,so no SiHCl_3 in the samples was demonstrated by comparing with the spectrum of standard sample of high-purity SiCl_4(99.9999%).Furthermore,the absorption peak of -OH at 3700～3500 cm~(-1) was analyzed quantitatively.As the polarity of CCl_4 is similar to SiCl_4 ,it was choosen as matrix solution.Triphenyl silanol was choosen as standard sample.The results showed correlation coefficient is 0.9963,molar absorptivity ε=108 L·mol~(-1)·cm~(-1), the content of-OH was analyzed quantitatively.