Stabilisation of water-in-oil emulsions to improve - eTheses ...

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2.11 Characterisation & Analysis of microcrystalline structure ........................... 37 2.11.1 Rheology & Texture ........................................................................... 37 2.11.2 Differential Scanning Colorimetry - DSC ........................................... 39 2.11.3 Pulsed Nuclear Magnetic Resonance – pNMR ................................. 40 2.11.4 Cryogenic Scanning Electron Microscopy - Cryo-SEM ..................... 41 3 Materials ........................................................................................................... 42 3.1 Waxes & Emulsifiers .................................................................................. 42 3.2 Emulsifier Selection ................................................................................... 42 3.2.1 Emulsifier Blend Calculations ............................................................... 44 4 Research Methodology ..................................................................................... 45 4.1 Differential Scanning Colourimetry – DSC & Enthalpy calclations ............. 45 4.2 Sample Formulation 1 - Basic Lipstick Preparation .................................... 47 4.3 Interfacial Tension and Surface Excess Concentration .............................. 48 4.3.1 IFT Plate Measurement principle .......................................................... 51 4.4 Sample Formulation 2 - Emulsion Lipstick Preparation .............................. 52 4.5 Pulsed Nuclear Magnetic Resonance – pNMR; Emulsion stability & Droplet size distribution ..................................................................................................... 54 4.5.1 Droplet Size Distribution measurement ................................................ 57 4.6 Microscopy ................................................................................................. 58 4.6.1 Optical Microscopy ............................................................................... 58 4.6.2 Cryo-Scanning Electron Microscopy – Cryo-SEM ................................ 59 4.7 Texture Profile Analysis - TA ..................................................................... 60 iv
4.7.1 Penetrometer Test ................................................................................ 60 4.7.2 Compression Test ................................................................................ 62 4.7.3 Rheology .............................................................................................. 64 5 Results, Data Analysis & Discussion ................................................................. 65 5.1 Introduction ................................................................................................ 65 5.2 Interfacial tension ....................................................................................... 65 5.3 Thermo-physical Characteristics using Differential Scanning Colorimetry – DSC on Raw Waxes & Basic Lipstick Formula ..................................................... 73 5.3.1 Thermo-physical Characteristics – DSC on Waxes .............................. 73 5.3.2 Wax selection for Simplified Basic Lipstick Formula & Thermo-physical Characteristics – DSC Basic Lipstick Formula .................................................. 74 5.3.3 Thermo-physical Characteristics – DSC on Emulsions ........................ 76 5.4 Emulsion Stability ....................................................................................... 83 5.4.1 Coalescence and Droplet Evolution ...................................................... 83 5.5 Emulsifier, Droplet Size Distribution & Microscopy .................................... 86 5.5.1 Size Distribution and Mophology .......................................................... 86 5.6 Texture Profile Analysis - TA ..................................................................... 99 5.6.1 Introduction ........................................................................................... 99 5.6.2 Penetration and Compression .............................................................. 99 5.7 Rheology .................................................................................................. 105 5.7.1 Introduction ......................................................................................... 105 5.7.2 Viscoelasticity ..................................................................................... 105 v
Page 1 and 2: Stabilisation of water-in-oil emuls
Page 3 and 4: Abstract The stabilisation of water
Page 5: Contents 1 Introduction ...........
Page 9 and 10: Figures Fig. 1.1. The global cosmet
Page 11 and 12: Fig. 5.18. DSC Thermograms for the
Page 13 and 14: Fig. 5.36. Changes in the viscoelas
Page 15 and 16: Table. 5.6. Emulsion based Lipstick
Page 17 and 18: Symbols α Alpha β Beta β’ Beta
Page 19 and 20: provide additional moisture for the
Page 21 and 22: 1.1 Layout of the Thesis This Thesi
Page 23 and 24: more than 2 to 3 applications daily
Page 25 and 26: O HO O C H 3 CH 3 O OH O O O Molecu
Page 27 and 28: C H 3 HO O OH Molecular Formula = C
Page 29 and 30: C H 3 C H 3 Molecular Formula = C 6
Page 31 and 32: the long chains. Due to its structu
Page 33 and 34: and subsequent infections. This can
Page 35 and 36: In order to attain a state of minim
Page 37 and 38: which there is an excess of opposit
Page 39 and 40: By applying the HLB system, one wil
Page 41 and 42: 2.7 Emulsion stability & instabilit
Page 43 and 44: (Voorhees, 1992; Dickinson, Ritzoul
Page 45 and 46: chains are in free rotation and pre
Page 47 and 48: (a) (b) (c) Fig. 2.7. Double chain
Page 49 and 50: prevented by the addition of crysta
Page 51 and 52: 2.9 Microbial stability & Origin of
Page 53 and 54: There are a number of important fac
Page 55 and 56: which of course is an important con
Page 57 and 58:
ideal for assessing not only the de
Page 59 and 60:
3 Materials 3.1 Waxes & Emulsifiers
Page 61 and 62:
With the continuous phase being oil
Page 63 and 64:
melting point range in order to mai
Page 65 and 66:
The moulds were then placed in a fr
Page 67 and 68:
Table. 4.2. IFT Procedure settings
Page 69 and 70:
4.4 Emulsion Lipstick Preparation F
Page 71 and 72:
The water was transferred directly
Page 73 and 74:
emulsions were taken in triplicate
Page 75 and 76:
d0,0; number-weighted mean (e.g. NM
Page 77 and 78:
4.7 Texture Profile Analysis - TA T
Page 79 and 80:
4.7.2 Compression Test The second m
Page 81 and 82:
4.7.3 Rheology Rheological non-dest
Page 83 and 84:
critical micelle concentration (CMC
Page 85 and 86:
Interfacial Tension (mN/m) 10 CMC -
Page 87 and 88:
Sorbitan Hydrophilic portion (Water
Page 89 and 90:
HO O O O O Water droplet O O O O HO
Page 91 and 92:
5.3.2 Wax selection for Simplified
Page 93 and 94:
5.3.3 Thermo-physical Characteristi
Page 95 and 96:
Heat Flow Endo/Exo (mW) 2% PGPR DSC
Page 97 and 98:
Heat Flow Endo/Exo (mW) 2% Span 80
Page 99 and 100:
Table. 5.3. Thermo-physical charact
Page 101 and 102:
Relative frequency Emulsion Stabili
Page 103 and 104:
drainage and rupture. In spite of t
Page 105 and 106:
Table. 5.4. Emulsion based Lipstick
Page 107 and 108:
Page 109 and 110:
Page 111 and 112:
the emulsification process along wi
Page 113 and 114:
Fig. 5.29. 30 wt% water content wit
Page 115 and 116:
Fig. 5.33. Cryo-SEM micrograph of H
Page 117 and 118:
no doubt give rise to a much denser
Page 119 and 120:
Table. 5.9. Texture profile penetro
Page 121 and 122:
Table. 5.10. Compression firmness d
Page 123 and 124:
Although no emulsions were prepared
Page 125 and 126:
G' & G'' (Pa) x 10 5 Viscoelastic p
Page 127 and 128:
Table. 5.11. Viscoelastic moduli, G
Page 129 and 130:
potentially reduce microbial spoila
Page 131 and 132:
Appendix The following Figures; 5.9
Page 133 and 134:
Heat Flow Endo/Exo (mW) 5 4 3 2 1 0
Page 135 and 136:
Heat Flow Endo/Exo (mW) 2.0 1.5 1.0
Page 137 and 138:
References Adamczyk, S., Lázaro, R
Page 139 and 140:
Dweck, A. C., & Burnham, C. A. M. (
Page 141 and 142:
Kobayashi, H., & Tagami, H. (2004).
Page 143 and 144:
Pourreza, N., & Rastegarzadeh, S. (
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