A method for the determination of carbon tetrachloride(CCl4)in refined titanium tetrachloride(TiCl4)by gas chromatography with ECD after hydrolysis under acid suppression was developed.Hydrolysis reactions were carried out according to the ratio(S/V)of TiCl4 to the hydrolysis solution(2 mol/L HCl)as 1∶5,and CCl4 in hydrolysis solutions was extracted with nonane.The results showed that CCl4 added to hydrolysis solutions of high pure TiCl4 could be almost extracted with recoveries of 92.3%-101%,and the HCl concentration in range of 0.85-6 mol/L presented no effects on extracted recoveries.Furthermore,hydrolysis solutions could maintain the stable condition of clarifying while S/V≤1∶4.The recoveries of CCl4 added to high pure TiCl4 were in the range of 87.6%-115% with RSDs of 4.2%-8.5%.The method showed good accuracy and stability.The quantitation limit of the method for 5 mL refined TiCl4 sample was 6.80 μg/L,which was far below the limited value of foreign advanced standards for CCl4 in refined TiCl4.