标准加入法定量测定四氯化钛中的三氯乙酰氯

Quantitaive determination for the trichloro-acetyl chloride in titanium tetrachloride by means of standard addition extrapolation

建立了一种定量测定精四氯化钛中的杂质三氯乙酰氯的方法 ,在国内尚属首次。本方法采用自制的专用红外密封池 ,用标准加入法获得一系列精四氯化钛的红外谱图 ,绘制标准曲线 ,外推得到精四氯化钛中所含三氯乙酰氯的含量 ,方法简便。三氯乙酰氯的最低测定限为 1× 10 -4 % ,符合朗伯 -比耳定律的范围为 0～ 0 85mg/mL ,加纯物质回收率为 94%～ 10 6 % ,多次测定的相对标准偏差为 9% ,因此此方法有较好的精密度和准确度 ,完全能满足监控精四氯化钛中所含这种杂质的要求。

In this paper,a method has been designed for determination of the trichloro acetyl chloride in titanium tetrachloride.The content of trichloro acetyl chloride in TiCl 4 is determined by a self made infrared sealed cell,using the standard addition extrapolation method.Within a limit of 1×10 -4 % and in the range of 0～0.85 mg/ml,it conforms to the Lambert Beer formulas.The average recovery of additing pure is 94～106%,RSD=9%.This method is precise and repetitive.