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Microemulsion and Macroemulsion Behaviour of Systems Containing Oil

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Microemulsion and Macroemulsion Behaviour of Systems Containing Oil THE UNIVERSITY OF HULL MICROEMULSION AND MACROEMULSION BEHAVIOUR OF SYSTEMS CONTAINING OIL, WATER AND NONIONIC SURFACTANT being a Thesis submitted for the Degree of Doctor of Philosophy in the University of Hull by N David Ian Horsup, B. Sc. August 1991 ACKNOWLEDGEMENTS I would like to express my sincere gratitude to my supervisor, Dr. Paul Fletcher for his assistance -and advice during the period of my research and for his encouragement of my interest in surface and colloid chemistry. Thanks are also due to Dr. Robert Aveyard, Dr. Bernard Binks and my fellow colleagues for many fruitful discussions. I am also grateful to the Agricultural and Food ResearchCouncil and Unilever (Colworth) for the provision of a three year studentship. August 1991 To my parentsfor providing me with the opportunity to pursue my academicstudies. Scientist atoneis tracepoet, fiegives us the moon,he promises the stars, he'fI makpus a new universeif it comesto that. Allen Ginsberg, "Poem Rocket, " Kaddish and Other Poems (1961). ABSTRACT In this thesis, attempts have been made to correlate some equilibrium properties of microemulsions with the formation and stability of macroemulsions. Studies have been mainly limited to water-in-oil (W/O) systems stabilised by pure nonionic (CnE, Initially however, brief surfactantsof the poly-oxyethylene alkyl ether n) type. a accountis presentedof the behaviour of W/O microemulsions stabilised by commercial nonionic surfactantsof the type usedin foods. A detailed study of the equilibrium behaviour of W/O microemulsions stabilised by tetra-oxyethylene mono-n-dodecyl ether, C12E4,in hydrocarbon oils is presented. Aggregates form above a certain surfactant concentration in the oil, designated the critical microemulsion concentration, cµc. Changes in the monolayer curvature induced through changing the temperature,salt concentration and the nature of the oil phase,are discussedin terms of an effective surfactant molecular geometry.The effect of solubilisation of protein into the dispersedaqueous phase is also presented. The corresponding W/O macroemulsions prepared with these systems at concentrations in excess of the cµc breakdown primarily by droplet sedimentation. There appears to be an optimum surfactant concentration at which maximum stabilisation is achieved. This is approximately equal to the cµc of the surfactant in the oil phase. Addition of microemulsion droplets to the oil dramatically increases the rate of oil phase resolution. For a fixed concentration of aggregated surfactant, the acceleration rate is rather insensitive to the size of the microemulsion droplets. These findings are reasonably consistent with a depletion flocculation mechanism in which microemulsions are assumed to behave as hard spheres and are excluded from the intervening region between approaching emulsion droplets. Microemulsion phase behaviour is also reported for oil phases containing different concentrationsof medium and long chain length triglycerides (MCT, LCT) in heptane. The critical microemulsion concentration is observedto increasedramatically 1 upon increasing the concentration of triglyceride. Additionally, the enthalpy change upon transfer of a mole of C12E4monomers from the oil phase to the preferred microemulsion droplet curvature becomes significantly less exothermic as the concentrationof MCT in the oil phaseincreases. The breakdown of W/O macroemulsions produced with these triglyceride systems is also consistent with a depletion flocculation mechanism. Emulsions prepared with 75% MCT as the oil phase undergo coalescence once an approximately close- packed droplet volume fraction is achieved. It is shown that as the cµc increases (through the addition of MCT or increasing the temperature), the stability of the emulsion dramatically decreases. Using a technique of time-resolved fluorimetry, the rate of exchange of probe molecules between microemulsion droplets has been determined. The exchange rate is always slowest at the solubilisation phase boundary where inter-droplet attractions are a minimum. The rate constants at this phase boundary are similar for aggregates formed in both heptane and in an equal volume ratio mixture of heptane : MCT. The possible relevance to the magnitude of the exchange rate constant of energies associated with bending the surfactant monolayer and desorbing surfactant from the droplet surface are considered. This technique has also been applied to three surfactant systems for which monolayer bending rigidities have previously been reported. Microemulsion exchange rates measuredat equivalent positions on the solubilisation phaseboundary increaseas the monolayer rigidity decreases. The stability of the corresponding W/O macroemulsionsis also observed to follow this order, the fastest water resolution rates being observedfor the systemswith the lowest monolayer rigidities. 11 PUBLICATIONS The work contained within this thesis has given rise to the following publications: (1) Chapters5&7. Effect of microemulsif:ed surfactant in destabilising water-in- oil emulsionscontaining C12E4.B. P. Binks, P.D. I. Fletcher and D. I. Horsup. Accepted for publication in Colloids and Surfaces. (2) Chapter 6. Droplet dynamics in water-in-oil microemulsions and macroemulsionsstabilised by nonionic surfactants. Correlation of measuredrates with monolayer bending elasticity. P.D. I. Fletcher and D. I. Horsup. Submitted to the Journal of the Chemical Society, FaradayTransactions. ill GLOSSARY ol Some of the abbreviations and terms used in this thesis are given below. Others defined locally are within the text. - A areaper surfactantmolecule within a planar oil-water interface a emulsion droplet radius A. area per surfactant molecule at the interface between the droplet core and the surfactantmonolayer Ah effective area of a surfactant head group within a curved microemulsion interface A, effective area of a surfactant tail group within a curved microemulsion interface AOT di-ethylhexyl sodium sulphosuccinate BSA bovine serum albumin C concentrationof aggregatedsurfactant in g/cm3 cmc critical micelle concentration cµc critical microemulsion concentration CnEm nonionic surfactantof the polyoxyethylene alkyl ether type C.P. cloud point a-CT a-chymotrypsin D apparentdiffusion coefficient D. diffusion coefficient at infinite particle dilution G Gibbs free energy G(t) intensity autocorrelationfunction HLB hydrophile-lipophile balance i generalindex for componenti iv Ia fluorescenceintensity at time t= zero fluorescenceintensity at time t j auxiliary index for all componentsother than the ith K monolayer bending rigidity constant K Gaussian curvature elastic modulus kB Boltzmann's constant k, ý secondorder rate constantfor the exchangeof probe moleculesbetween microemulsion droplets kac secondorder diffusion controlled rate constant ko first order fluorescenceintensity decayrate constant kq first order fluorescence intensity decay rate constant for a microemulsion droplet containing a single quencher molecule kt first order rate constantfor microemulsion droplet exchange LCT long chain length triglyceride M molecular weight MCT medium chain length triglyceride m, surfactantconcentration MV methyl viologen N averagenumber of protein moleculesper microemulsion droplet NA Avogadro's constant Nagg number of surfactant molecules constituting one micelle/microemulsion n refractive index ni number of moles of speciesi O/W oil-in-water (microemulsion/macroemulsion) P geometricalpacking factor p as a subscript denotespressure All osmotic pressure V Q magnitudeof the scatteringvector r general abbreviation for a microemulsion droplet radius RB ruthenium tris-bipyridyl rc microemulsion core radius ro spontaneousradius of curvature r1 principal radius of curvature rH microemulsion hydrodynamic radius R molar gas constant R0j1 mole ratio of dispersed oil to total surfactant Rwatar mole ratio of dispersed water to total surfactant R' mole ratio of dispersedcomponent to surfactantwithin an aggregate R'oa mole ratio of dispersed oil to surfactant within a microemulsion droplet R'wawr mole ratio of dispersed water to surfactant within a microemulsion droplet t an arbitrary time T* temperatureat which the oil-water interfacial tension is a minimum tx% time for x% resolution of oil or water SDS sodium dodecyl sulphate T temperature (absolute or Celsius specified in text) Va general volume specified in the text Vd depletion flocculation interaction energy Vi molecular volume of speciesi W/O water-in-oil (microemulsion/macroemulsion) [x], average number of quenchers in aggregates containing excited fluorescentprobes in the steady-statephase of the fluorescencedecay [A] concentrationof speciesA V1 a first virial coefficient of the apparent diffusion coefficient 7 general symbol for the tension at an oil (or air) - water interface 7c interfacial tension at a surfactant concentration in excess of the cmc or cµc 5 effective surfactant interfacial film thickness 0 volume fraction of droplets r, interfacial surfaceexcess concentration of surfactant 11 viscosity P density x wavelength of light (j) angular velocity vii CONTENTS Chapter Title Page One INTRODUCTION. THE BEHAVIOUR OF SURFACTANTS IN OIL-WATER MIXTURES 1 1.1 Surfactantsin Solution 1 1.1.1 What are surfactants ? 1 1.1.2 Surfactants in water 2 1.13 Surfactants in oils 8 1.2 9 Surfactantsin Oil-Water Mixtures - Microemulsions 1.2.1 One phase oil-water mixtures 9 1.2.2 Multi phase oil-water mixtures 13 1.23 Surfactant geometryand monolayer curvature ideas 15 1.2.4 Oil-water interfacial
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