Determination of Carbon Tetrachloride in Refined Titanium Tetrachloride

KeyWord:titanium tetrachloride  carbon tetrachloride  gas chromatography  suppression hydrolysis

Abstract:

      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¡Ã5,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¡Ü1¡Ã4.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 ¦Ìg/L,which was far below the limited value of foreign advanced standards for CCl4 in refined TiCl4.