S. Levin et al., CHARACTERIZATION OF SUBMICROMETER EMULSIONS USING SEDIMENTATION FIELD-FLOW FRACTIONATION WITH POWER FIELD PROGRAMMING, Analytical chemistry, 66(3), 1994, pp. 368-377
Sedimentation field-flow fractionation (SdFFF), operated with power-ba
sed field programming, was shown to be effective in the characterizati
on of submicrometer fat emulsions. Field programming, in which the dec
rease of field strength with time gradually increases the average velo
city of the sample components, extends the capabilities of sedimentati
on field-flow fractionation in handling polydisperse samples. Submicro
meter fat emulsions were analyzed by three different rates of field de
cay and two different initial field strengths, using various stop-now
times. Identical size distribution profiles were obtained under all ci
rcumstances, using the appropriate stop-flow times. Fractions were col
lected from the SdFFF eluting bands, and diameters were analyzed by ph
oton correlation spectroscopy, showing good agreement with values give
n by the FFF instrument. The agreement between the two methods indicat
ed also that polydispersity of size dominated band broadening. Accurat
e and highly reproducible size distribution profiles were obtained in
all the cases studied. Sample loadability was examined by studying ove
rloading effects and detection limits. The linearity of detector respo
nse was also established, by injecting increasing loads of sample. The
accuracy of the FFF peak shape was examined experimentally, by collec
ting fractions, dissolving the emulsion in them, and measuring the UV
absorption of the solutions. The profile formed by the fractions was r
elatively close to the FFF band, proving that light scattering does no
t seriously distort the size distribution profile.