Characterization of Microemulsions using Small Angle Scattering Techniques

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1 Characterization of Microemulsions using Small Angle Scattering Techniques Dissertation zur Erlangung des akademischen Grades doctor rerum naturalium (Dr. rer. nat.) vorgelegt der Mathematisch-Naturwissenschaftlich-Technischen Fakultät (mathematisch-naturwissenschaftlicher Bereich) der Martin-Luther-Universität Halle-Wittenberg von Herrn Anuj Shukla geb. am 10. März 1973 in Sitapur (Indien) Gutachter: 1. Prof. Dr. Heinrich Graener 2. Prof. Dr. Reinhard Neubert 3. Dr. habil. Wolf-Dieter Hergeth Halle (Saale), den urn:nbn:de:gbv: [http://nbn-resolving.de/urn/resolver.pl?urn=nbn%3ade%3agbv%3a ]

2 ii CONTENTS Contents 1. Introduction What is a microemulsion (ME)? What does a ME droplet look like? What is dynamic behavior of ME droplet? Design of MEs Applications of MEs 5 2. Small Angle Scattering Techniques Comparison of Scattering Techniques and 6 the Length Scales which they Probe 2.2. Light Scattering Small Angle Neutron Scattering (SANS) Theoretical Background Static Light Scattering (SLS) from Interacting ME Droplets Dynamic Light Scattering (DLS) Monodisperse, Non-Interacting ME Droplets Polydisperse, Interacting ME Droplets Volume Fraction Dependence of Diffusion Coefficient SANS from Interacting ME Droplets The Form Factor The Structure Factor & Pair Distribution Function 29

3 CONTENTS iii 3.7. Interdroplet Interaction Data Acquisition and Treatment Data Acquisition: Static and Dynamic Light Scattering Data Treatment: SLS Data Treatment: DLS Data Acquisition and Treatment: SANS Results And Discussion Water AOT n- Alkanes MEs Layered Sphere Model Droplet Size and Polydispersity Refractive Index Increment DLS Results SLS Results Interdroplet Interactions and Droplet size SANS and CONTIN Results SLS Results DLS Results Shape Fluctuations of ME 70 Droplets with Increasing Temperature 5.2. Characterization of Pharmaceutical MEs Interdroplet Interaction and Droplet Size 73 of O/W - MEs of Pharmaceutical Interest DLS Results 74

4 iv CONTENTS Effect of Proposed Interdroplet Interaction 76 on the Stability of O/W - MEs Behavior of Each Constituent Solubilized 79 in MEs of Pharmaceutical Interest O/W MEs of Pharmaceutical Interest MEs with Different Ratios of Water/PG MEs with Different Amounts of Oil Effect of Drug Incorporation MEs with Different Kinds of Oils DLS Results SANS Results Effect of Temperature on ME Droplet W/O MEs of Pharmaceutical Interest Different Ratios of Span 20/ Tween MEs with Different Ratios of Water/DMSO MEs with Different amounts of Surfactant MEs with Different Kinds of Oils Effect of Temperature on ME Droplets Characterization of MEs having Local Anaesthetics 94 as Dispersed Phase Interdroplet Interaction Different Amount of colloidal Phase Effect of ph Summary and Conclusions / Zusammenfassung und 97 Schlussfolgerungen 6.1. Model ternary water/aot/n-alkanes MEs 97

5 CONTENTS v 6.2. MEs of pharmaceutical interest 99 Suggestions for Future Studies I Appendix A II Appendix B VII Appendix C IX Appendix D XII List of References XVI

6 vi CONTENTS List of Abbreviations AOT AOT-MEs DLS DMSO EMLA EO Eutanol HLB HNC HS IPM IPP ME NMR OA O/W PO Poloxamer 331 PG PY SANS SAS SLD SLS Span 20 Tagat O2 Tween 80 W/O Sodium bis(2-ethylhexyl) sulfosuccinate (Aerosol - OT) Water/AOT/n-alkanes Systems Dynamic Light Scattering Dimethyl sulfoxide Eutectic Mixture of Local Anaesthetics Ethylene Oxide 2-Octyl-1-dodecanol Hydrophilic-Lipophilic-Balance Hypernetted-Chain Hard Sphere Isopropyl myristate Isopropyl palmitate Microemulsion Nuclear Magnetic Resonance Oleic acid Oil-in-Water Propylene Oxide Polyoxyethylene Polyoxypropylene Block co-polymer Propylene Glycol Percus-Yevick Small Angle Neutron Scattering Small Angle Scattering Scattering Length Density Static Light Scattering Sorbitan monolaurate Polyoxyethylene glycerol monooleate Polyoxyethylene sorbitan mono-oleate Water-in- Oil

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