K. Kovacshadady et T. Varga, A SYSTEMATIC STUDY OF IMPREGNATION OF THIN-LAYERS WITH DIFFERENT ION-PAIRING REAGENTS AND BY DIFFERENT METHODS, JPC. Journal of planar chromatography, modern TLC, 8(4), 1995, pp. 292-299
The efficiency of a variety of techniques used for impregnation of sil
ica gel layers with tetramethylammonium bromide (TMA), tetrabutylammon
ium bromide (TBA), cetyltrimethylammonium bromide (CTMA), and trioctyl
methylammonium chloride (TOMA) has been determined. The absolute conce
ntrations of the different ion-pairing reagents on the layers were mea
sured by spectrophotometry, potentiometry, and thermogravimetry. When
development-type impregnations were used, a concentration gradient was
observed on the layer in the direction of the development. The slope
of the gradient depended on the impregnation technique used and the na
ture of the ion-pairing reagent. Smoother gradients were obtained by u
se of overdevelopment than by impregnation by other types of developme
nt, e.g. development up to a given distance in a saturated or unsatura
ted chamber, or by use of OPLC or a sandwich chamber. Horizontal and v
ertical dipping by use of an immersion device resulted in almost unifo
rm distribution of the reagent on the layer. The concentrations of the
ion-pairing reagents on the lever increased with increasing dipping t
ime, except for CTMA-impregnated layers, for which longer dipping time
s resulted in desorption. The retention and resolution of model compou
nds reflected the concentration of ion-pairing reagents in the station
ary phase.