Bs. Broyles et al., Visualization of solute migration in chromatographic columns - Influence of the frit porosity, J CHROMAT A, 917(1-2), 2001, pp. 1-22
The dual-perspective, on-column detection method previously described was u
sed to observe the effects of the inlet frit on the profiles of chromatogra
phic bands. Visualization of bands of iodine was achieved by injecting its
dilute solutions in carbon tetrachloride into a glass column packed with a
C-18-bonded silica and eluted with carbon tetrachloride, which has the same
refractive index as the packing material. The bands were photographed on-c
olumn with two standard 35-mm SLR cameras oriented at right angle. The phot
ographs were scanned and the digitized images of the sample bands analyzed
with proper software. A number of columns, as similar as possible, were fit
ted with different 2- and 10-mum porosity stainless steel frits. Subsequent
analysis of the digitized band images revealed irregularities in the band
shape resulting from frit contributions to band dispersion. The 2-mum frits
produced more dramatic effects overall than the coarser frits. Local axial
dispersion coefficient values, expressed as local reduced plate height, we
re calculated. The results demonstrate the possibly damaging effects of the
frit on the band shape. (C) 2001 Elsevier Science B.V. All rights reserved
.