ABSTRACT
The simplest field flow fractionation technique, which uses the earth's gravity as the external field is applied to isolate two populations, which differ in both shape and size, from a polydisperse sub-micron TiO2 powder of homogenous density. The fraction eluted first is spherical with an average diameter of 0.31 microm while the second fraction is ellipsoidal and can be associated with a 0.45 microm hydrodynamic diameter. Elution conditions appeared to be very sensitive to electrolyte and surfactant characteristics in the carrier phase as well as on the sample concentration. Using 25 microl (1%, w/w) sample suspension, separations of spherical from ovoid particles was performed in almost 2 h with a mobile phase of 0.001 M KNO3-0.01% (v/v) Fl-70 in water in a 0.025-cm thick channel made of polystyrene walls.
Subject(s)
Chemical Fractionation/methods , Titanium/isolation & purification , Gravitation , Particle SizeABSTRACT
Sedimentation field flow fractionation (SdFFF) operated at multi gravitational field is used to analyse a highly polydisperse TiO2 colloidal suspension. From the initial sample, time dependent eluted fractions are collected and submitted to electron microscopy (EM) shape and size analysis. To assess the accuracy of FFF in determining the average size of the different fractions, these are re-introduced into the channel by means of two different procedures, the on-channel concentration of the fractions and the direct re-injection of pre-concentrated fractions (DRI). Both methods appear accurate to determine the average size of every fraction, associated to a lower recovery in the case of DRI. The fractogram band spreading characteristics of the re-introduced fractions are correlated to the particle size distribution measured by EM. After density determination of fractionated particles, the fractogram is calibrated in terms of size and size distribution using data obtained from EM for each fraction. Quantitative analyses, based on particle counting showed high recovery (80-90%) of the eluted species. However, this loss limited the possibility to extend signal information to a quantitative one.
Subject(s)
Titanium/chemistry , Chemical Fractionation , Microscopy, ElectronABSTRACT
The complex conductivity of concentrated TiO(2) suspensions (up to 50 vol%) was measured over a large frequency range (1 MHz-1.8 GHz), as a function of grain volume content. These measurements highlight relaxation phenomena in the intermediate frequency range, which are associated with the dispersed powder. These phenomena were previously noted in O'Brien's theoretical developments. A quantitative data analysis was made, in terms of time constant distribution, using the CONTIN software, from Provencher. As a result, a complex process is highlighted, including two main mechanisms in different ranges of time constants. Particularly, we showed good agreement between the higher frequency mechanism and the O'Brien theory. From Dukhin's lambda ratios, which are ratios of grain surface to bulk electrolyte conductances, we calculated the electrolyte conductivity as a function of powder concentrations. At higher powder concentrations, these values are different from those measured with centrifuged liquids. Copyright 2000 Academic Press.
