Comparative TEM of Freeze-fractured Colloidal Liquid Aphrons and Conventional Emulsions

Extract

Colloidal Liquid Aphrons (CLAs) are composed of surfactant doped non-aqueous inner cores surrounded by thin surfactant films. These are created by intense stirring of the non-aqueous phase in an aqueous surfactant solution. Large interfacial areas, due to small size, and high stability (much greater than conventional emulsions) make aphron dispersions attractive for a variety of mass transfer limited processes. The unusual stability of CLA dispersions has been attributed to the multi-layered structure that includes an entrapped water shell around the non-aqueous core as postulated by Sebba. However, no direct evidence for the structure of the surfactant-stabilized interface surrounding the CLAs has been previously published.

CLAs were prepared as previously reported. Comparative conventional emulsions were made similarly, with the lipid phase free of the Tergitol^®(15-S-3) surfactant used in the CLAs. Aliquots (≈30 μl) of the dispersions were spread on 0.15 mm thick, 10 mm diameter copper supports These supports were ultra-rapidly frozen via plunging in liquid propane(−190°C). The frozen samples were inserted onto a pre-cooled rotary stage of a freeze-etch unit (modified Balzers BA-510) and fractured by knife at 150°C with a residual pressure of approx. 6.5 x 10⁻⁵ Pa. The replicas were shadowed with ≈2nm of Pt at 30° followed by 10-15 nm of carbon by arc evaporation. The resulting replica was washed in an 10% graded isopropanol series, rehydrated, washed in chromic acid, rinsed in de-ionized H₂O, and then mounted on 300 mesh grids. TEM was performed on a JEOL 100CX operated at 120keV.