精四氯化钛中痕量四氯化碳的分析  

Determination of Carbon Tetrachloride in Refined Titanium Tetrachloride

作　　者：陈江韩[1] 郭鹏然[1] 陈智勇[1] 宋化灿[1] 牟德海[1] 

机构地区：[1]中国广州分析测试中心广东省分析测试技术公共实验室,广东广州510070

出　　处：《分析测试学报》2013年第7期829-833,共5页Journal of Instrumental Analysis

基　　金：科技部创新方法工作专项资助项目(2011IM030700)

摘　　要：建立了酸抑制水解-气相色谱法(GC-ECD)分析精四氯化钛中痕量CCl4的方法。以2 mol/L盐酸为酸抑制水解溶液,四氯化钛与水解溶液按样液比(S/V)1∶5进行水解反应,水解液用正壬烷连续萃取3次。结果表明,水解液中加标的CCl4基本被萃取完全,萃取回收率为92.3%～101%,盐酸浓度在0.85～6mol/L范围内对萃取结果无影响;S/V≤1∶4时,水解体系保持稳定澄清透明状态。高纯四氯化钛加标样中CCl4的加标回收率为87.6%～115%,样品分析的相对标准偏差为4.2%～8.5%,方法准确性和稳定性较好。该方法对5 mL精四氯化钛样品中CCl4的定量下限为6.80μg/L,远低于国外精四氯化钛中CCl4的限定标准。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.

关 键 词：四氯化钛 四氯化碳 气相色谱法 抑制水解 

分 类 号：O657.71[理学—分析化学]