RESUMO
Physically meaningful characterization of irregularly shaped particles continues to present substantial challenges to the experimentalist. "Equivalent diameters" based on experimental techniques such as static and dynamic light scattering or sedimentation have proliferated to the point that they are often no longer recognized as equivalent. This study demonstrates the use of dual-fluid disk centrifuge photosedimentometry coupled with rheological measurements of viscosity to provide direct insights into both the average mass of a structured particle size distribution and the average hydrodynamic diameter.
RESUMO
Disc centrifuge photosedimentometry (DCP) with fluids of different densities is used to simultaneously determine the particle size and effective density of spherical silica particles. Incorporation of a calibrated infrared pyrometer into a DCP instrument is shown to enhance the measurement capability of the DCP technique by correcting for the temperature dependence of the spin fluid's density and viscosity. Advantages of absolute DCP determinations for size and density analysis relative to standardized DCP measurements include the elimination of instrument standardization with a particle of known density and measurements or estimation of the effective particle density. The reliability of diameter determinations provided by absolute DCP was confirmed using silica particles with nominal diameters ranging from 250 to 700 nm by comparison of these analyses with a diameter determination by transmission electron microscopy for silica particle size standards. Effective densities determined by absolute DCP for the silica particles ranged from 2.02 to 2.34 g/cm(3). These findings indicate that the silica particles have little or no porosity. The reported characterization of colloidal silica using absolute DCP suggests applicability of the technique to a variety of particle types including colloidal materials other than silica, core-shell particles, compositionally heterogeneous mixtures of nanoparticles, and irregularly shaped, structured colloids.