高效液相色谱法同时测定反应物中的单氯代苯酐及单氯代邻苯二甲酸  

Simultaneous Determination of Monochlorophthalic Anhydride and Monochlorophthalic Acid in Substrates by High Performance Liquid Chromatography

作　　者：袁秀伶[1] 

机构地区：[1]天津大学石油化工技术开发中心,天津300072

出　　处：《色谱》2006年第5期495-498,共4页Chinese Journal of Chromatography

摘　　要：采用高效液相色谱法同时测定了化学反应物中的3-氯代苯酐、4-氯代苯酐、3-氯代邻苯二甲酸、4-氯代邻苯二甲酸。样品在80～100℃下用无水乙醇酯化。色谱分析条件：色谱柱为Luna—C18柱，流动相为甲醇-0．15mol／L磷酸二氢铵溶液（体积比为42：58），检测波长为240nm，外标法定量。方法简便、快速，具有良好的精密度、回收率和线性关系，A high performance liquid chromatographic method has been developed for the simultaneous determination of 3-chlorophthalic anhydride, 4-chlorophthalic anhydride, 3-chlorophthalic acid and 4-chlorophthalic acid. The operating conditions were a Luna-C18 column at 30 ×, methanol-0. 15 mol/L ammonium dihydrogen phosphate solution （42： 58, v/v） as mobile phase with flow rate of 0. 8 mL/min, ultra-violet detection at 240 nm. An external standard method was used. Samples were esterified with absolute ethanol at 80 - 100 ℃ for 15 min. 3- Chlorophthalic anhydride and 4-chlorophthalic anhydride were respectively converted to two isomers of monochloro-O-carboxyl ethyl benzoate, and the monochlorophthalic acids were not esterified under the reaction conditions. The results demonstrated that the recoveries were 99. 1% - 101.5% ; the relative standard deviations ranged from 0.48% to 0.87% ; the linear ranges were 3. 12 -312.4 mg/L, 2.96 -222.3 mg/L, 1.86 - 186.4 mg/L, 1.41 - 141.0 mg/L for 3- chlorophthalic anhydride, 4-chlorophthalic anhydride, 3-chlorophthalic acid and 4-chlorophthalic acid, respectively. The method was simple, accurate and fast. The six components could be separated completely in about 20 min.

关 键 词：高效液相色谱法 3-氯代苯酐 4-氯代苯酐 3-氯代邻苯二甲酸 4-氯代邻苯二甲酸 

分 类 号：O658[理学—分析化学]