The formation of colloids by the controlled reduction, nucleation, and growth of inorganic precursor salts in different media has been investigated for more than a century. Recently, the preparation of ultrafine particles has received much attention since they can offer highly promising and novel options for a wide range of technical applications (nanotechnology, electrooptical devices, pharmaceutics, etc). The interest derives from the well-known fact that properties of advanced materials are critically dependent on the microstructure of the sample. Control of size, size distribution and morphology of the individual grains or crystallites is of the utmost importance in order to obtain the material characteristics desired. Several methods can be employed for the synthesis of nanoparticles. On the one hand, the reduction can occur in diluted aqueous or alcoholic solutions. On the other hand, the reduction process can be realized in a template phase, e.g. in well-defined microemulsion droplets. However, the stability of the nanoparticles formed mainly depends on their surface charge and it can be influenced with some added protective components. Quite different types of polymers, including polyelectrolytes and amphiphilic block copolymers, can for instance be used as protecting agents. The reduction and stabilization of metal colloids in aqueous solution by adding self-synthesized hydrophobically modified polyelectrolytes were studied in much more details. The polymers used are hydrophobically modified derivatives of poly(sodium acrylate) and of maleamic acid copolymers as well as the commercially available branched poly(ethyleneimine). The first notable result is that the polyelectrolytes used can act alone as both reducing and stabilizing agent for the preparation of gold nanoparticles. The investigation was then focused on the influence of the hydrophobic substitution of the polymer backbone on the reduction and stabilization processes. First of all, the polymers were added at room temperature and the reduction process was investigated over a longer time period (up to 8 days). In comparison, the reduction process was realized faster at higher temperature, i.e. 100°C. In both cases metal nanoparticles of colloidal dimensions can be produced. However, the size and shape of the individual nanoparticles mainly depends on the polymer added and the temperature procedure used. In a second part, the influence of the prior mentioned polyelectrolytes was investigated on the phase behaviour as well as on the properties of the inverse micellar region (L2 phase) of quaternary systems consisting of a surfactant, toluene-pentanol (1:1) and water. The majority of the present work has been made with the anionic surfactant sodium dodecylsulfate (SDS) and the cationic surfactant cetyltrimethylammonium bromide (CTAB) since they can interact with the oppositely charged polyelectrolytes and the microemulsions formed using these surfactants present a large water-in-oil region. Subsequently, the polymer-modified microemulsions were used as new templates for the synthesis of inorganic particles, ranging from metals to complex crystallites, of very small size. The water droplets can indeed act as nanoreactors for the nucleation and growth of the particles, and the added polymer can influence the droplet size, the droplet-droplet interactions, as well as the stability of the surfactant film by the formation of polymer-surfactant complexes. One further advantage of the polymer-modified microemulsions is the possibility to stabilize the primary formed nanoparticles via a polymer adsorption (steric and/or electrostatic stabilization). Thus, the polyelectrolyte-modified nanoparticles formed can be redispersed without flocculation after solvent evaporation. / Die Bildung von Kolloiden durch kontrollierte Reduktion, durch Keimbildung und durch Wachstum anorganischer Precurser in unterschiedlichen Medien wird seit mehr als einem Jahrhundert intensiv beforscht. Vor kurzem hat die Herstellung ultrafeiner Partikel viel Aufmerksamkeit errungen, da sich hieraus vielversprechende neue Möglichkeiten für ein breites Spektrum an technischen Anwendungen (Nanotechnologie, elektrooptische Materialen, Pharmazeutik, usw.) ergeben. Das Interesse leitet sich von der weithin bekannten Tatsache ab, dass die Eigenschaften der „advanced materials“ von der Mikrostruktur der Probe deutlich abhängig sind. Die gezielte Steuerung der Größe, der Größenverteilung und der Morphologie der einzelnen Keime oder Kristallite ist von größter Wichtigkeit, um die gewünschten Eigenschaften zu erreichen. Verschiedene Methoden können für die Synthese von Nanopartikel verwendet werden. Einerseits kann eine Reduktion in verdünnten wässrigen oder alkoholischen Lösungen stattfinden, andererseits kann der Reduktionsprozess in einer Templatphase, z.B. in definierten Mikroemulsionströpfchen stattfinden. Die Stabilität der produzierten Nanopartikel hängt hauptsächlich von ihrer Oberflächenladung ab, welche durch schützende Komponenten zusätzlich beeinflusst werden kann. Verschiedene Arten von Polymeren, einschließlich Polyelektrolyte und amphiphile Blockcopolymere, können als solche Komponenten benutzt werden. Die Reduktion und Stabilisierung von Metallkolloiden in der wässrigen Lösung durch Addition von hydrophob modifizierten Polyelektrolyten werden bereits ausführlich studiert. Die verwendeten Polymere sind hydrophob modifizierte Derivate des Natrium-Polyacrylat, der Maleinsäure Copolymere sowie das verzweigte Poly(ethylenimin). Erstaunlicherweise genügt bereits die Anwesenheit die verwendeten Polyelektrolyte zu Reduzierung und Stabilisierung der Goldnanopartikel. Darüber hinaus wurde der Einfluss der hydrophoben Seitenkette des Polymer auf den Reduktions- und Stabilisierungsprozess bei unterschiedliche Reaktionstemperatur untersucht. In beiden Fällen können Metallnanopartikel kolloidaler Größe hergestellt werden, jedoch hängt die Größe und die Form der einzelnen Nanopartikel hauptsächlich vom dem zugefügten Polymer und vom verwendeten Temperaturverfahren ab. Im zweiten Teil wurde der Einfluss der vorher erwähnten Polyelektrolyte auf das Phaseverhalten sowie auf die Eigenschaften der inversen mizellaren Region (L2 Phase) der quaternären Systeme untersucht, die aus einem Tensid, Toluol-Pentanol – Gemisch (1:1) sowie Wasser bestehen. Dabei wurden hauptsächlich ionische Tenside, wie z.B. das anionische Natriumdodecylsulfate (SDS) und das kationische Cetyltrimethylammonium-bromid (CTAB) verwendet, da sie mit den geladenen Polyelektrolyten wechselwirken können. Darüber hinaus wurden die polymer-modifizierten Mikroemulsionen als neue Template für die Synthese von anorganischen Nanopartikeln verwendet. Die Wassertröpfchen können in der Tat als Nanoreaktoren für die Keimbildung und das Wachstum der Partikel dienen, und das zugefügte Polymer kann die Tröpfchengröße, die Tröpfchen-Tröpfchen Wechselwirkungen, sowie die Stabilität des Tensidfilms durch Polyelektrolyt-Tensid Komplexbildung beeinflussen. Ein weiterer Vorteil der polymer-modifizierten Mikroemulsionen ist die Stabilizierung der produzierten Primärteilchen über eine Polymeradsorption (durch sterische bzw. elektrostatische Stabilisierung), welche eine Redispergierung der Polyelektrolyte-modifiziert Nanopartikel, nach Lösungsmittel-verdampfung, ohne Aggregation der Partikel erlaubt.

NMR methods have been designed and employed in studying ofcomplex liquids and solids formed by surfactants. PGSE NMRexperiments are easily biased by convection; this artifact canbe avoided by changing the sample holder and by usingconvection-compensated pulse sequences. The temperaturedistribution within samples was controlled using thetemperature dependent order parameter for CBr2H2dissolved in a thermotropic nematic solvent.Electronic ringing that often spoils accurate NMR experimentsfor broad lines was removed by the using composite pulses andquadrupole echo sequences with appropriate phase cycles. Field-dependent81Br and35Cl NMR relaxation studies in micellar solutions ofC16TAX surfactants showed that the structure ordynamics of the hydration shell is more influenced by thesurfactant cation for bromide than for chloride, in agreementwith their position in the Hoffmeister series. The presence ofa small but significant frequency-dependent relaxation showedthat the lateral self diffusion of the anions may be reduced ascompared to its bulk value in diluted solutions but only with afactor of 1.0 - 2.5. The ions are clearly not "bound" to thesurface. A field-dependent2H NMR relaxation study on the CTABr-α-d2and benzene-d6showed an initial one-dimensional micellargrowth followed by the appearance of microemulsion droplets onaddition of benzene. The local mobility of the benzene wasreduced when solubilized in small amounts, consistent with aninitial average location of benzene at the micellar interface.The surfactant diffusion coefficients fromconvection-compensated PGSE NMR experiments in the C12E8-D2O system showed monotonous growth of the micellesupon increasing temperature. Emulsion droplets in the C12E5-decane-D2O system where shown to coarsen according to theOstwald ripening theory after being brought out of equilibriumby a temperature drop. X-ray scattering and2H NMR line-shape and relaxation experimentssuggested that complex solids formed by a partly-sulfatedpolysaccharide and CnTAB exhibit regular ordering at both microscopicand mesoscopic length scales. <b>Keywords</b>: CTAB, CTAC, C12E8, C12E5, decane, benzene, CBr2H2, polysaccharide, micelle, microemulsion, emulsion,Ostwald ripening, NMR,81Br,35Cl,2H, field- dependent spin relaxation, PGSE, selfdiffusion, convection, ringing, thermometer, generalized Blochequations, EXORCYCLE, quadrupole echo, SAXS, WAXS, cryo-TEM.

The purpose of this research was to develop the pseudo-ternary phase diagrams for a model drug delivery system consisting of vitamin E (model drug) + soybean oil + surfactant + co-surfactant (anhydrous glycerol) + water. The model drug (vitamin E) was loaded in the oil phase. The effects of different surfactants (pure and mixed) on the phase diagram, especially the microemulsion region, were investigated. The influence of drug loading level on the phase diagram was also determined. The surfactants studied were Tween 20, Tween 80, Cremopher EL, and their mixtures. The size (area) of the microemulsion region of the phase diagram was found to be dependent on the type of surfactant used and the loading level of drug (vitamin E). The phenomenon of phase inversion from W/O microemulsion to O/W microemulsion was also investigated for the drug delivery system consisting of soybean oil (0% w/w Vitamin E loading or 30% w/w Vitamin E loading) + Tween 80 + anhydrous glycerol + water. The inversion of phases was detected by observing changes in the viscosity of the system.

The purpose of this research was to develop the pseudo-ternary phase diagrams for a model drug delivery system consisting of vitamin E (model drug) + soybean oil + surfactant + co-surfactant (anhydrous glycerol) + water. The model drug (vitamin E) was loaded in the oil phase. The effects of different surfactants (pure and mixed) on the phase diagram, especially the microemulsion region, were investigated. The influence of drug loading level on the phase diagram was also determined. The surfactants studied were Tween 20, Tween 80, Cremopher EL, and their mixtures. The size (area) of the microemulsion region of the phase diagram was found to be dependent on the type of surfactant used and the loading level of drug (vitamin E). The phenomenon of phase inversion from W/O microemulsion to O/W microemulsion was also investigated for the drug delivery system consisting of soybean oil (0% w/w Vitamin E loading or 30% w/w Vitamin E loading) + Tween 80 + anhydrous glycerol + water. The inversion of phases was detected by observing changes in the viscosity of the system.

<p>NMR methods have been designed and employed in studying ofcomplex liquids and solids formed by surfactants. PGSE NMRexperiments are easily biased by convection; this artifact canbe avoided by changing the sample holder and by usingconvection-compensated pulse sequences. The temperaturedistribution within samples was controlled using thetemperature dependent order parameter for CBr₂H₂dissolved in a thermotropic nematic solvent.Electronic ringing that often spoils accurate NMR experimentsfor broad lines was removed by the using composite pulses andquadrupole echo sequences with appropriate phase cycles.</p><p>Field-dependent⁸¹Br and³⁵Cl NMR relaxation studies in micellar solutions ofC₁₆TAX surfactants showed that the structure ordynamics of the hydration shell is more influenced by thesurfactant cation for bromide than for chloride, in agreementwith their position in the Hoffmeister series. The presence ofa small but significant frequency-dependent relaxation showedthat the lateral self diffusion of the anions may be reduced ascompared to its bulk value in diluted solutions but only with afactor of 1.0 - 2.5. The ions are clearly not "bound" to thesurface. A field-dependent²H NMR relaxation study on the CTABr-α-<i>d</i><i>2</i>and benzene-<i>d</i><i>6</i>showed an initial one-dimensional micellargrowth followed by the appearance of microemulsion droplets onaddition of benzene. The local mobility of the benzene wasreduced when solubilized in small amounts, consistent with aninitial average location of benzene at the micellar interface.The surfactant diffusion coefficients fromconvection-compensated PGSE NMR experiments in the C₁₂E₈-D₂O system showed monotonous growth of the micellesupon increasing temperature. Emulsion droplets in the C₁₂E₅-decane-D₂O system where shown to coarsen according to theOstwald ripening theory after being brought out of equilibriumby a temperature drop. X-ray scattering and²H NMR line-shape and relaxation experimentssuggested that complex solids formed by a partly-sulfatedpolysaccharide and C_nTAB exhibit regular ordering at both microscopicand mesoscopic length scales.</p><p><b>Keywords</b>: CTAB, CTAC, C₁₂E₈, C₁₂E₅, decane, benzene, CBr₂H₂, polysaccharide, micelle, microemulsion, emulsion,Ostwald ripening, NMR,⁸¹Br,³⁵Cl,²H, field- dependent spin relaxation, PGSE, selfdiffusion, convection, ringing, thermometer, generalized Blochequations, EXORCYCLE, quadrupole echo, SAXS, WAXS, cryo-TEM.</p>

Reservoir pressure and solution gas can significantly alter the microemulsion phase behavior and the design of a surfactant-polymer flood. This dissertation shows how to predict changes in microemulsion phase behavior from dead oil at atmospheric pressure to live crude at reservoir pressure. Our method requires obtaining only a few glass pipette measurements of microemulsion phase behavior at atmospheric pressure. The key finding is that at reservoir pressure the optimum solubilization ratio and the logarithm of optimal salinity behave linearly with equivalent alkane carbon number (EACN). These trends are predicted from the experimental data at atmospheric pressure based on density calculations of pure components using the Peng-Robinson equation-of-state (PREOS). We show that predictions of the optimum conditions for live oil are in good agreement with the few experimental measurements that are available in the literature. We also present new measurements at atmospheric pressure to verify the established trends. The experiments show that while pressure induces a phase transition from upper microemulsion (Winsor Type II+) to lower microemulsion (Winsor Type II-), solution gas does the opposite. An increase in pressure decreases the optimum solubilization ratio and shifts the optimum salinity to a larger value. Adding methane to dead oil at constant pressure does the reverse. Thus, these effects are coupled and both must be taken into account. We show using a numerical simulator that these changes in the optimum conditions can impact oil recovery if not accounted for in the SP design. / text

It is estimated that the shallow reservoirs of Ugnu, West Sak and Shraeder Bluff in the North Slope of Alaska hold about 20 billion barrels of heavy oil. The proximity of these reservoirs to the permafrost makes the application of thermal methods for the oil recovery very unattractive. It is feared that the heat from the thermal methods may melt this permafrost leading to subsidence of the unconsolidated sand (Marques 2009; Peyton 1970; Wilson 1972). Thus it is necessary to consider the development of cheap non-thermal methods for the recovery of these heavy oils. This study investigates non-thermal techniques for the recovery of heavy oils. Chemicals such as alkali, surfactant and polymer are used to demonstrate improved recovery over waterflooding for two oils (A:10,000cp and B:330 cp). Chemical screening studies showed that appropriate concentrations of chemicals, such as alkali and surfactant, could generate emulsions with oil A. At low brine salinity oil-in-water (O/W) emulsions were generated whereas water-in-oil (W/O) emulsions were generated at higher salinities. 1D and 2D sand pack floods conducted with alkali surfactant (AS) at different salinities demonstrated an improvement of oil recovery over waterflooding. Low salinity AS flood generated lower pressure drop, but also resulted in lower oil recovery rates. High salinity AS flood generated higher pressure drop, high viscosity emulsions in the system, but resulted in a greater improvement in oil recovery over waterfloods. Polymers can also be used to improve the sweep efficiency over waterflooding. A 100 cp polymer flood improved the oil recovery over waterflood both in 1D and 2D geometry. In 1D geometry 1PV of polymer injection increased the oil recovery from 30% after waterflood to 50% OOIP. The tertiary polymer injection was found to be equally beneficial as the secondary polymer injection. It was also found that the combined application of AS and polymer did not give any major advantage over polymer flood or AS flood alone. Chemical EOR technique was considered for the 330cp oil B. Chemical screening studies showed that microemulsions could be generated in the system when appropriate concentrations of alkali and surfactant were added. Solubilization ratio measurement indicted that the interfacial tension in the system approached ultra-low values of about 10-3 dynes/cm. The selected alkali surfactant system was tested in a sand pack flood. Additionally a partially hydrolyzed polymer was used to provide mobility control to the process. The tertiary injection of ASP (Alkali-Surfactant-Polymer) was able to improve the oil recovery from 60% OOIP after the waterflood to almost 98% OOIP. A simple mathematical model was built around viscous fingering phenomenon to match the experimental oil recoveries and pressure drops during the waterflood. Pseudo oil and water relative permeabilities were calculated from the model, which were then used directly in a reservoir simulator in place of the intrinsic oil-water relative permeabilities. Good agreement with the experimental values was obtained. For history matching the polymer flood of heavy oil, intrinsic oil-water relative permeabilities were found to be adequate. Laboratory data showed that polymer viscosity is dependent on the polymer concentration and the effective brine salinity. Both these effects were taken into account when simulating the polymer flood or the ASP flood. The filtration theory developed by Soo and Radke (1984) was used to simulate the dilute oil-in-water emulsion flow in the porous media when alkali-surfactant flood of the heavy oil was conducted. The generation of emulsion in the porous media is simulated via a reaction between alkali, surfactant, water and heavy oil. The theory developed by Soo and Radke (1984) states that the flowing emulsified oil droplets clog in pore constrictions and on the pore walls, thereby restricting flow. Once captured, there is a negligible particle re-entrainment. The simulator modeled the capture of the emulsion droplets via chemical reaction. Next, the local water relative permeability was reduced as the trapping of the oil droplets will reduce the mobility of the water phase. This entrapment mechanism is responsible for the increase in the pressure drop and improvement in oil recovery. The model is very sensitive to the reaction rate constants and the oil-water relative permeabilities. ASP process for lower viscosity 330 cp oil was modeled using the UTCHEM multiphase-multicomponent simulator developed at the University of Texas at Austin. The simulator can handle the flow of three liquid phases; oil, water and microemulsion. The generation of microemulsion is modeled by the reaction of the crude oil with the chemical species present in the aqueous phase. The experimental phase behavior of alkali and surfactant with the crude oil was modeled using the phase behavior mixing model of the simulator. Oil and water relative permeabilities were enhanced where microemulsion is generated and interfacial tension gets reduced. Experimental oil recovery and pressure drop data were successfully history matched using UTCHEM simulator. / text

Developing hybrid processes for heavy oil recovery is a major area of interest in recent years. The need for such processes originates from the challenges of heavy oil recovery relating to fluid injectivity, reservoir heating, and oil displacement and production. These challenges are particularly profound in shaley thin oil deposits where steam injection is not feasible and other recovery methods should be employed. In this work, we aim to develop and optimize a hybrid process that involves moderate reservoir heating and chemical enhanced oil recovery (EOR). This process, in its basic form, is a three-stage scheme. The first stage is a short electrical heating, in which the reservoir temperature is raised just enough to create fluid injectivity. After electrical heating has created sufficient fluid injectivity, high-rate high-pressure hot water injection accelerates the raise in temperature of the reservoir and assists oil production. At the end of hot waterflooding the oil viscosities are low enough for an Alkali-Co-solvent-Polymer (ACP) chemical flood to be performed where oil can efficiently be mobilized and displaced at low pressure gradients. A key aspect of ultra-low IFT chemical flood, such as ACP, is the rheology of the microemulsions that form in the reservoir. Undesirable rheology impedes the displacement of the chemical slug in the reservoir and results in poor process performance or even failure. The viscosity of microemulsions can be altered by the addition of co-solvents and branched or twin-tailed co-surfactants and by an increase in temperature. To reveal the underlying mechanisms, a consistent theoretical framework was developed. Employing the membrane theory and electrostatics, the significance of charge and/or composition heterogeneity in the interface membrane and the relevance of each to the above-mentioned alteration methods was demonstrated. It was observed that branched co-surfactants (in mixed surfactant formulations) and temperature only modify the saddle-splay modulus (k ̅) and bending modulus (k) respectively, whereas co-solvent changes both moduli. The observed rheological behavior agrees with our findings. To describe the behavior of microemulsions in flow simulations, a rheological model was developed. A key feature of this model is the treatment of the microemulsion as a bi-network. This provides accuracy and consistency in the calculation of the zero-shear viscosity of a microemulsion regardless of its type and microstructure. Once model parameters are set, the model can be used at any concentration and shear rate. A link between the microemulsion rheological behavior and its microstructure was demonstrated. The bending modulus determines the magnitude of the viscous dissipations and the steady-shear behavior. The new model, additionally, includes components describing the effects of rheology alteration methods. Experimental viscosity data were used to validate the new microemulsion viscosity model. Several ACP corefloods showing the large impact of microemulsion viscosity on process performance were matched using the UTCHEM simulator with the new microemulsion rheology model added to the code. Finally, numerical simulations based on Peace River field data were performed to investigate the performance of the proposed hybrid thermal-chemical process. Key design parameters were identified to be the method of heating, duration of the heating, ACP slug size and composition, polymer drive size, and polymer concentration in the polymer drive. An optimization study was done to demonstrate the economic feasibility of the process. The optimization revealed that short electrical heating and high-rate high-pressure waterflooding are necessary to minimize the energy use and operational expenses. The optimum slug and polymer drive sizes were found to be ~0.25 PV and ~1 PV, respectively. It was shown that the well costs dominate the expenditure and the overall cost of the optimized process is in the range of 20-30 $⁄bbl of incremental oil production. / text

Living radical polymerization has proved to be a powerful tool for the synthesis of polymers as it allows for a high degree of control over the polymer microstructure and the synthesis of tailored molecular architectures. Although it has great potential, its use on an industrial scale is limited due to environmental and economical aspects. Nitroxide mediated polymerization is explored to bring this technology closer to adoption in commercial applications. One of the obstacles encountered using nitroxide mediated polymerization in microemulsion systems is the difficulty in controlling both the particle size and target molecular weight. Due to the nature of the formulation, a decrease in the target molecular weight is coupled to an increase in the particle size. For many applications, it is important to be able to design polymer particles with both specifications independently. Strategies to decouple these two properties and processing conditions required for targeting a range of particle sizes and molecular weights for n butyl acrylate latexes are presented. Furthermore, in an attempt to reduce the large amounts of surfactant typically used in microemulsions, these methods were explored at low surfactant to monomer ratios (0.2 to 0.5 by wt.) in order to reduce the costs associated with excess surfactant and post processing steps for surfactant removal (high surfactant levels also give poor water-resistance in coatings). Stable nanolatexes with particle sizes <40 nm have been obtained by other groups using NMP in microemulsions with SG1 but have done so by using much higher surfactant to monomer ratios (~2.5 by wt.) and at much lower solids content (6 10 wt. %). In this work, molecular weights of 20,000 to 80,000 g∙mol-1 were targeted and stable, n-butyl acrylate microemulsions with particle sizes ranging from 20 120 nm were prepared at a solids content of 20 wt. % using much lower surfactant concentrations. Although numerous studies have shown the effects of process parameters on particle sizes and methods to control the molecular weight, the decoupling of the molecular weight and particle size effect in NMP microemulsions under these conditions has not been done to this extent. In copolymer systems, nitroxide mediated polymerization also provides an efficient method to synthesize well defined block copolymers. Random copolymers are widely used as protective colloids, but the use of block copolymers for these applications has not been well studied. It is unclear what effects do the importance of a narrow molecular weight distribution and purity of block copolymers have on their performance as protective colloids. In order to investigate this, a range of block copolymers with different properties would need to be synthesized for systematic analysis. The direct synthesis of polystyrene b poly(acrylic acid) copolymers of varying lengths and compositions was successful by use of nitroxide mediated polymerization in bulk and solution polymerization. The characterization of these amphiphilic block copolymers was explored by titration and nuclear magnetic resonance spectroscopy. / Thesis (Master, Chemical Engineering) -- Queen's University, 2012-09-28 15:43:00.513

A multidisciplinary literature survey revealed that copolymeric nanoparticles could be applied in various technologies such as the production of paint, adhesives, packaging material and lately especially drug delivery systems. The specialized application and investigation of copolymers in drug delivery resulted in the synthesis of two series of copolymeric materials, i.e. poly(styrene-co-methyl methacrylate) (P(St-co-MMA)) and poly(styrene-co-ethyl methacrylate) (P(St-co-EMA)) were synthesized via the technique of o/w microemulsion copolymerization. These copolymers have not as yet been utilized to their full potential in the development of new drug delivery systems. However the corresponding hydrophobic homopolymer poly(styrene) (PS) and the hydrophilic homopolymer poly(methyl methacrylate) (PMMA) are known to be biocompatible. Blending of homopolymers could result in novel applications, however is virtually impossible due to their unfavorable mixing entropies. The immiscibility challenge was overcome by the synthesis of copolymers that combined the properties of the immiscible homopolymers. The synthesized particles were analyzed by gel permeation chromatography combined with multi-angle laser light scattering (GPC-MALLS) and attenuated total reflectance Fourier infrared spectroscopy (ATR-FTIR). These characterizations revealed crucial information to better understand the synthesis process and particle properties i.e. molecular weight, nanoparticle size and chemical composition of the materials. Additionally, GPC-MALLS revealed the copolymer chain conformation. These characterizations ultimately guided the selection of appropriate copolymer nanoparticles to develop a controlled-release drug delivery system. The selected copolymers were dissolved in a pharmaceutically acceptable solvent, tetrahydrofuran (THF) together with a drug, rifampin. Solvent casting of this dispersion resulted in the evaporation of the solvent and assembly of numerous microscale copolymer capsules. The rifampin molecules were captured in these microcapsules through a process of phase separation and coacervation. These microcapsules finally sintered to produce a multi-layer film with an unusual honeycomb structure, bridging yet another size scale hierarchy. Characterization of these delivery systems revealed that both series of copolymer materials produced films capable of controlling drug release and that could also potentially prevent biofilm adhesion. / Thesis (Ph.D. (Pharmaceutics))--North-West University, Potchefstroom Campus, 2008.