ISSN:
1612-1112
Keywords:
Gas chromatography
;
Glass capillaries
;
Chirasil-Val
;
Immobilisation
;
Enantiomeric separation
Source:
Springer Online Journal Archives 1860-2000
Topics:
Chemistry and Pharmacology
Notes:
Summary Immobilisation methods of the chiral silicone stationary phase Chirasil-L-Val have been studied. In addition to the standard techniques of radical-induced immobilisation with dicumyl peroxide and azo tert-butane, immobilisation was solely achieved by thermal treatment: conditioning at low flow-rates or under stop-flow conditions led to unexpectedly high immobilisation despite mild temperatures. The presence of water vapor in the carrier gas accelerated the immobilisation process. While up to 75% immobilisation was attainable with both ATB and thermal methods, immobilisation with DCUP did not exceed 50%, despite relatively high DCUP concentrations. Whilst all immobilisation methods were accompanied by varying degrees of racemisation at the chiral centre, it was possible to establish conditions that yielded a high immobilisation (in excess of 70%) with a negligible loss in enantiomeric selctivity. The immobilisation reactions also slightly affected the polarity of the stationary phase, reflected in a shift of the Kovats-Indices of amino acid derivatives and in the accompanying “Squalane-Effect”. With respect to immobilisation, racemisation and polarity shift, thermal immobilisation with water-saturated carrier gas proved to be the optimum method.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1007/BF02268157
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