Font Size: a A A

Synthesis Of New Pelysiloxanes As GC Stationary Phase And Its Chromatographic Performance Evaluation

Posted on:2012-12-14Degree:MasterType:Thesis
Country:ChinaCandidate:Y H GaoFull Text:PDF
GTID:2211330338965383Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
In this paper, two new polysiloxane GC stationary phases were synthesized by the Diels-Alder reaction and the hydrosilylation reaction. The chromatography performance of stationary phases were evaluated.Diphenyl phenyl polysiloxane stationary phases:firstly, the polymethylvinylsilox-ane with different content of vinyl(10%,20%,30%) were prepared, and then the 2,5-dimethyl-3,4-diphenylcyclopenta-2,4-dienone and 2-ethyl-3,4-diphenylcyclopen-ta-2,4-dienone were synthesized. Finally, the 2,5-dimethyl-3,4-diphenylcyclopenta-2, 4-dienone and 2-ethyl-3,4-diphenylcyclopenta-2,4-dienone were dissolved in dry dip-henyl ether, the diphenyl phenyl polysiloxane were obtained, which were polysiloxane as main chain and diphenyl phenyl as side chain. A small amount of vinyl was residued by control the feed ratio, and the stationary phase can be used of cross-linked column to improve the temperature resistance.The new stationary phases were coated on the capillary columns by the static method, and the performances of the columns were evaluated. The new stationary phases demonstrated high column efficiency and good temperature resistance, the substituted benzene and polycyclic aromatic mixtures can be separated well on these columns. The new columns can be used for analysis of environmental pollutants.Ester and ether polysiloxane stationary phases:firstly, the dimethylpolysiloxane was synthesized and the trifluoromethanesulfonic acid as catalyst, the part of the hy-drogen of dimethylpolysiloxane was synthesized by hydrolysis reaction. The allyl et-hyl ether,ethyl undecylenate and anethole were grafted to the polysiloxane. The allyl ethyl ether and ethyl undecylenate were grafted to the different contents of dim-ethylpolysiloxane by the ratio of 1:1. The ester and ether polysiloxane, which were polysiloxane as main chain and ester,ether as side chain.The new stationary phases were coated on the capillary columns by the static method, and the performances of the columns were evaluated. The allyl ethyl ether polysiloxane and ethyl undecylenate polysiloxane stationary phases can easily coated, owned good temperature resistance. The columns have better selectivity in the analysis of alcohols,esters and white spirit. The new columns can be used for analysis of alcohols,esters,ethyl,aldehyde and ketone. The anethole polysiloxane stationary phases should be inerted before coating, the new stationary phases demonstrated high column efficiency and good temperature resistance. The alcohols,esters and substituted benzene can be separated on the new columns. The new columns can be used for analysis of white spirit and substituted benzene.
Keywords/Search Tags:Gas Chromatography, Capillary Column, Stationary Phase, polysiloxane, Chromatographic Performance
PDF Full Text Request
Related items