Analytical Methods Of P-toluenesulfonic Acid Isomers

AB STRACT The first part of this thesis is about gas chromatography analysis of the qualitative and quantitative determination of toluenesulphonic acid (TSA)isomers. I A single-step method for the preparation of TSA ethyl esters by reaction with triethyl orthoformate.Water is removed by azeotropic distillation of the sample solution in toluene prior to the addition of the reagent,and the reaction mixture can be injected into gas chromatograph without further purification. The present work was to develop a fast and reliable method.The analysis may be performed on the QF- 1 packed column under isothermal conditions and the analysis condition of gas chromatography was optimized.A new internal standard C21 was used.Moremover,we also studied the preparing of toluensulfonic acid isomers in different tempreature range and scoutted the ratio of the para, ortho and meta isomers during the esterification. At last,the faction of disturb the quantitative analytical have been discussed,such as esterify time,injection port temperature etc.If we can control those influence factor carefully,a good conclusion of detect TSA isomers will be achieved.This method is of great value in TSA isomers analysis because it is quick and accurate. In the second part of this thesis , the chromatographic characteristics of Porapak QS stationary phases has been evaluated.This column packing materials provide sharp,symmetrical peaks and low retention volumes for water, alcohols,free fatty acids,esters etc. For this kind of stationary phase has the long retention time during it is detected the McReynolds constants at 120 C .Besides,the peak of gas chromatography has serious tailing.We measured the McReynolds constants at 170 慍 column temperature for the first time,and put forward the relationship of column temperature and retention time,plate number and column temperature. We also determined the TG and DTA of Porapak QS stationary phases in N2 and Air, Ill 3 and the maximum limit temperature was obtained. These reserch have important guide sense for this kind of stationaiy phase when we research the mechanism of thermodynamics between the separate component and Porapak QS stationary pbase.In addition,these research have important value in application and development of this stationary phase.