Preparation And Properties Of Gas - Phase Capillary Column Based On Modified

Capillary gas chromatography is one of the important means of the modern chromatographic separation and analysis,because of its advantages of fast,high efficiency and high sensitive. With the development of science and society, people pay more attention to food safety and environmental protection. Because people need to close boiling, complex compounds with the similar structure analysis and separated. Chromatography researchers need to study more excellent gas chromatography stationary phase with high column efficiency, good thermal stability,high selectivity to meet the practical requirements of phase analysis. Cucurbiturils(Q[n],n=5,6,7,8) is supramolecular chemistry relay crownethers, cyclodextrins and calixarenes after a highly anticipated a novel class of synthetic macrocyclic host molecules caged. It has been widely studied in the field of molecular assembly,moolecular recognition and supramolecular catalysis.However, as gas chromatography stationary pahase area is still rarely report.In this paper,(OH)10Q[5] as gas chromatography stationary phase to prepare a capillary column by sol-gel. Homemade capillary column for the separation properties,chemical stability, thermal stability, pillars pole and the efficiency of the column were investigated. The main contents are as follows:1、Research progress of gas chromatography stationary phases review.2、Synthesis and separation and purification of cucurbiturils(Q[n],n=5,6,7,8),using nuclear magnetic resonance techniques(NMR) to characterize. Then Q [5] on the basis of references improved synthesis of(OH)10Q[5], using the method of column chromatography to separate and purify. Infrared Spectroscopy(IR), NMR were used to characterize the target compound.3、Prepared the PDMS/(OH)10Q[5] capillary column gas phase by sol-gel, and for evaluation of its performance. This column coating is dense and uniform, no cracks, the thickness is about 1μm. It has good chemical stability, thermal stability and reproducibility, △I=575, belong to the weak poar column, column efficiency 487plate/m. In the Optimization the chromatographic conditions, the column of alkanes,alcohols, ketones, esters, amines, phenols six compounds were separated and measured, the result showed that the separation effect of chromatographic column is good for this six compounds.Three isomers of nitroaniline and two-dimethylphenol isomers also have good separation ability. The gas chromatography capillary column can effectively separated containing 2-pentanone, pentanol, n-decane, n-undecane,n-octanol, 2,6-dimethylphenol, methyl decanoate, methyl undecanoate, methyl laurate,4-nitroamline, ten kinds of compounds mixed samples.4 、 We use a sol-gel method of three chromatographic column polarity and behavior of chromatographic separation were compared, such as bonding PDMS/(HO)10Q[5] capillary column, non-bonding PDMS/Q[5] capillary column as well as blank PDMS capillary column without contain. Experimental results show that adding(HO)10Q[5] in PDMS can really improve the separation selectivity of chromatographic column, and due to the chromatographic column is the cause of chemical bonding, so chromatographic column has good chemical stability and thermal stability.But the inadequacies of the chromatographic column is the column efficiency is low, which may be related to the columns in the(HO)10Q[5] poor solubility and columns is not uniform caused.This is also for us to further improve the new column so the research direction and technical support in the future. The research provided the experimental basis and research direction for the future research of the gas chromatography stationary phase of cucurbiturils...