薄层色谱法分析十三碳二元酸及其单、双甲酯  

Determination of Tridecane Dicarboxylic Acid and Its Products of Esterification by Scanning Thin-Layer Chromatography

作　　者：王丽华[1] 齐邦峰[1] 王丽君[1] 

机构地区：[1]抚顺石油化工研究院,辽宁抚顺113001

出　　处：《石油化工高等学校学报》2003年第2期29-32,共4页Journal of Petrochemical Universities

摘　　要：　采用带有氢火焰离子化检测器的薄层色谱仪对十三碳二元酸,及其单甲酯和双甲酯进行了定性、定量的分析,较传统的毛细管气相色谱法及液相色谱法,具有重复性好、分离彻底及分析时间短的优点。根据十三碳二元酸,及其单甲酯和双甲酯极性不同,而沸点高的特点,选择二氯甲烷作为展开剂。为了提高分离度及防止拖尾现象的发生,而添加了少量的甲酸。达到最佳分离效果时,V二氯甲烷∶V甲酸=120∶0.5。考察了薄层色谱棒对样品的负载量,了解到每根色谱棒的最佳负载量应为10～30μg。为了提高方法的分析精度,又对点样、展开后的各组分的峰面积值的稳定性进行了考察,结果表明,至少在1.5h内,峰面积值没有变化。测出了每种组分的质量校正因子,分别为f双甲酯=1.00、f单甲酯=1.06、f二元酸=0.98。考察了方法的准确度和精密度,方法的相对误差≤2.1%。TLC/FID采用微量试样(几十微克),可分析相对分子质量高、极性差别大的组分。相对标准偏差≤2.3%,10个样品仅需1h。Qualitative and quantitative analytical method of analyzing tridecane dicarboxylic acid, its monomethyl ester and dimethyl ester by thin chromatograph with ionization detector of hydrogen flame is introduced. It is more advanced than the traditional capillary gas chromatography and liquid chromatography because of its good repeatability, complete separation, and short analytical time. According to the different polarity among tridecane dicarboxylic acid, monomethyl ester and its dimethyl ester as well as their high boiling point, dichloromethane was chosen as developed solvent. In order to raise their degree of separation and prevent the occurrence of dilatory tail, a little methanoic aid was added. The volume proportion of dichloromethane and methanoicacid should be Vdichloromethane∶Vmethanoicacid=120∶0.5 when separated completely. The loading of each chromatographic rod is investigated and the optimum loading was gotten, i.e.10～30 μg. The stability of each component's peak area is studied after finishing loading and developing, no change is shown at least within 1.5 hours. The mass calibration factor of each component is determined, fdi-ester=1.00, fmo-ester=1.05, fdi-acid=0.98.The accuracy and precision of this method is investigated and its relative error is no more than 2.1%. TLC/FID method needs only micro sample (teens of micrograms). The components with great relative molecular weight and high different polarity can be analyzed and its relative standard and derivation is no more than 2.3%. Only 1 hour is needed for ten samples' analysis.

关 键 词：薄层色谱法 十三碳二元酸 十三碳二元酸单甲酯 十三碳二元酸双甲酯 

分 类 号：TQ225.242[化学工程—有机化工] O657.7[理学—分析化学]