Harvey Scott D, Wenzel Thomas J
Pacific Northwest National Laboratory, National Security Directorate, MSIN: P7-07, 902 Battelle Boulevard, P.O. Box 999, Richland, WA 99352, USA.
J Chromatogr A. 2009 Sep 4;1216(36):6417-23. doi: 10.1016/j.chroma.2009.07.008. Epub 2009 Jul 15.
The purpose of this research was to investigate coating capillary columns with lanthanide(III) beta-diketonate polymers to provide gas-chromatographic columns with selectivity toward explosives and related compounds. Capillary columns were statically coated with a mixture of a lanthanide(III) beta-diketonate polymer, which utilized p-di(4,4,5,5,6,6,6-heptafluoro-1,3-hexanedionyl)benzene (dihed) as a ligand, and SE-30. A novel coating technique was developed that used a methanol-containing azeotrope to provide solubility for both polymers while maintaining a low boiling point compatible with static coating. As based on temperature-programmed retention indices, the experimental columns displayed selective retention of nitroaromatic, nitroalkane, and nitrate ester test probes relative to an appropriate SE-30 control column. Selective retention was more pronounced for strongest Lewis base analyte contained in the test mixture (i.e., cyclohexanone). Relative analyte retention on the La(dihed), Tb(dihed), and Eu(dihed) columns are discussed relative to Lewis acidity and solubility of the polymer in the azeotropic coating solution.
本研究的目的是研究用镧系(III)β-二酮聚合物涂覆毛细管柱,以提供对炸药及相关化合物具有选择性的气相色谱柱。毛细管柱用镧系(III)β-二酮聚合物(其使用对二(4,4,5,5,6,6,6-七氟-1,3-己二酮基)苯(二庚酮)作为配体)和SE-30的混合物进行静态涂覆。开发了一种新颖的涂覆技术,该技术使用含甲醇的共沸物为两种聚合物提供溶解性,同时保持与静态涂覆兼容的低沸点。基于程序升温保留指数,相对于合适的SE-30对照柱,实验柱对硝基芳烃、硝基烷烃和硝酸酯测试探针显示出选择性保留。对于测试混合物中所含最强路易斯碱分析物(即环己酮),选择性保留更为明显。相对于聚合物在共沸涂覆溶液中的路易斯酸度和溶解度,讨论了在La(二庚酮)、Tb(二庚酮)和Eu(二庚酮)柱上的相对分析物保留情况。