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| 1 | High-Resolution Optical and Confocal Microscopy | 1 |
| Olaf Hollricher and Wolfram Ibach | ||
| 1.1 | Introduction | 1 |
| 1.2 Introduction to Theoretical Considerations in High-Resolution | ||
| Microscopy | 3 | |
| 1.3 | Introduction to Confocal Microscopy | 3 |
| 1.4 | Electromagnetic Scattering in Optical Systems | 4 |
| 1.5 | 3D-Intensity Distribution in the Focus | 5 |
| 1.5.1 | Large Aperture Angles | 6 |
| 1.5.2 | Transition to Small Aperture Angles | 9 |
| 1.6 | Theory of Image Formation | 11 |
| 1.6.1 | Microscope | 11 |
| 1.6.2 | Confocal Microscope | 12 |
| 1.6.3 | Confocal Raman Microscope | 12 |
| 1.7 | Image Formation for Light Scattering | 13 |
| 1.7.1 | Scattering Point | 13 |
| 1.7.2 | Reflection at a Mirror | 15 |
| 1.8 | Image Formation for Raman Scattering | 16 |
| 1.8.1 | Raman Emitting Point | 16 |
| 1.8.2 | Raman Emission of a Layer | 17 |
| 1.9 | Pinhole Size | 18 |
| References | 20 | |
| 2 | Introduction to the Fundamentals of Raman Spectroscopy | 21 |
| Benjamin Dietzek, Dana Cialla, Michael Schmitt, and Jürgen Popp | ||
| 2.1 | Introduction | 21 |
| 2.2 | Classical Picture of Light Scattering | 22 |
| 2.2.1 | Frequency Dependence of Raman Scattering | 22 |
| 2.2.2 Classical "Selection Rule" and Comparison to IR | ||
| Absorption | 24 | |
| 2.2.3 | Scattered Raman Intensity | 25 |
| 2.2.4 | Shortfalls of the Classical Picture | 27 |
| 2.3 | Raman Cross-Section Enhancement Mechanisms | 27 |
| 2.3.1 | Resonant Raman Scattering | 28 |
| 2.3.2 Advantages and Applications of Resonance | ||
| Raman Scattering | 31 | |
| 2.3.3 | Surface-Enhanced Raman Scattering | 34 |
| References | 40 | |
| 3 | Raman Instrumentation for Confocal Raman Microscopy | 43 |
| Olaf Hollricher | ||
| 3.1 | Introduction | 43 |
| 3.2 | The Development of Raman Microscopes | 44 |
| 3.3 | Confocality | 45 |
| 3.4 | Throughput of a Confocal Raman Microscope | 46 |
| 3.4.1 | Laser Wavelength | 47 |
| 3.4.2 | Excitation Power | 47 |
| 3.4.3 | Objective | 48 |
| 3.4.4 | Microscope Throughput | 48 |
| 3.4.5 | Coupling Between Microscope and Spectrometer | 49 |
| 3.4.6 | Spectrometer Throughput | 49 |
| 3.4.7 | Gratings | 50 |
| 3.4.8 | CCD Detector | 51 |
| 3.5 | Conclusion | 60 |
| References | 60 | |
| 4 Software Requirements and Data Analysis in Confocal | ||
| Raman Microscopy | 61 | |
| Thomas Dieing and Wolfram Ibach | ||
| 4.1 | Introduction | 61 |
| 4.2 | Requirements for Data Acquisition Software | 62 |
| 4.2.1 | Data Acquisition | 62 |
| 4.2.2 | Correlation of Spatial and Spectral Data | 63 |
| 4.3 Description of the Data Sets Acquired in Confocal | ||
| Raman Microscopy | 65 | |
| 4.4 | Pre-processing of Raman Spectra | 66 |
| 4.4.1 | Cosmic Ray Removal | 66 |
| 4.4.2 | Smoothing | 68 |
| 4.4.3 Background Substraction and Subtraction | ||
| of Reference Spectra | 70 | |
| 4.5 | Image Generation | 72 |
| 4.5.1 | Univariate Image Generation | 72 |
| 4.5.2 | Multivariate Image Generation | 75 |
| 4.6 | Image Masks and Selective Average Calculation | 81 |
| 4.7 | Combination of Single Spectra with Multi-spectral Data Sets | 82 |
| 4.7.1 | Basis Spectra | 83 |
| 4.7.2 | Fitting Procedure | 83 |
| 4.8 | Combination of Various Images | 84 |
| 4.9 | The Law of Numbers | 85 |
| 4.10 | Materials and Methods | 88 |
| References | 89 | |
| 5 Nano-spectroscopy of Individual Carbon Nanotubes and Isolated | ||
| Graphene Sheets | 91 | |
| Alain Jungen | ||
| 5.1 | Introduction | 91 |
| 5.2 | Individual Carbon Nanotubes | 92 |
| 5.2.1 | Phonons | 92 |
| 5.2.2 | Theory | 95 |
| 5.2.3 | Experiment | 96 |
| 5.2.4 | Microscopy | 98 |
| 5.2.5 | Thermography | 100 |
| 5.3 | Isolated Graphene Sheets | 101 |
| 5.3.1 | Theory | 101 |
| 5.3.2 | Experiment | 102 |
| 5.3.3 | Charge Distributions | 105 |
| 5.4 | Conclusion | 107 |
| References | 108 | |
| 6 Raman Spectroscopy and Confocal Raman Imaging in Mineralogy | ||
| and Petrography...............................................Ill | ||
| Marc Fries and Andrew Steele | ||
| 6.1 Introduction..............................................Ill | ||
| 6.2 Raman Spectroscopy and Imaging as a Mineralogy/Petrography | ||
| Tool | 112 | |
| 6.2.1 | Working with Thin Sections | 114 |
| 6.2.2 | Control of Laser Power | 116 |
| 6.3 | "Raman Mineralogy" Using Imaging Raman Techniques | 119 |
| 6.3.1 | Mineral Phase Imaging | 120 |
| 6.3.2 | Crystallographic Orientation Imaging | 122 |
| 6.3.3 | Phase Composition Imaging | 123 |
| 6.4 | Examples of "Raman Petrography" Applications | 124 |
| 6.4.1 | Raman Analysis of Shocked Minerals | 124 |
| 6.4.2 | Contextual Imaging of Carbonaceous Materials | 126 |
| 6.4.3 | Fluid Inclusions | 129 |
| 6.4.4 | Ancient Terrestrial Carbonaceous Materials | 130 |
| 6.5 | Raman Mineralogy in Field Geology Studies | 130 |
| 6.5.1 | Extraterrestrial Exploration | 132 |
| 6.6 | Conclusion | 133 |
| References | 133 | |
| 7 Raman Micro-spectral Imaging of Cells and Intracellular Drug | ||
| Delivery Using Nanocarrier Systems | 137 | |
| Christian Matthaus, Tatyana Chernenko, Luis Quintero, Milos | ||
| Miljkovic, Lara Milane, Amit Kale, Mansoor Amiji, Vladimir | ||
| Torchilin, and Max Diem | ||
| 7.1 | Introduction | 137 |
| 7.2 | Method | 140 |
| 7.2.1 | Data Acquisition | 140 |
| 7.2.2 | Introduction to Data Processing Methods | 140 |
| 7.2.3 | Experimental | 144 |
| 7.3 | Results | 145 |
| 7.3.1 | Cell Imaging | 145 |
| 7.3.2 | Drug Delivery Systems | 152 |
| 7.4 | Discussion | 161 |
| References | 162 | |
| 8 | Confocal Raman Microscopy in Pharmaceutical Development | 165 |
| Thomas F. Haefele and Kurt Paulus | ||
| 8.1 | Introduction | 165 |
| 8.1.1 Vibrational Spectroscopy in Pharmaceutical | ||
| Development | 166 | |
| 8.1.2 | Imaging in Pharmaceutical Development | 169 |
| 8.1.3 | Chemical Imaging in Pharmaceutical Development | 172 |
| 8.1.4 Confocal Raman Microscopy in Pharmaceutical | ||
| Development | 176 | |
| 8.2 Applications of Confocal Raman Microscopy in Pharmaceutical | ||
| Development | 179 | |
| 8.2.1 | Practical Considerations | 179 |
| 8.2.2 Investigation of Solid Dosage Forms by Chemical | ||
| Imaging | 185 | |
| 8.3 | Conclusions | 198 |
| 8.4 | Materials and Methods | 198 |
| References | 199 | |
| 9 | Characterization of Therapeutic Coatings on Medical Devices | 203 |
| Klaus Wormuth | ||
| 9.1 | Background | 203 |
| 9.2 | Passive Therapeutic Coatings | 205 |
| 9.2.1 | Coating Thickness | 205 |
| 9.2.2 | Swelling of Hydrophilic Gel Coatings | 208 |
| 9.3 | Active Therapeutic Coatings | 210 |
| 9.3.1 | Coating Morphology | 210 |
| 9.3.2 Drug Mixed with Single Polymer: Morphology | ||
| andElution | 211 | |
| 9.3.3 Drug Mixed with Two Polymers: Blending | ||
| and Layering | 216 | |
| 9.3.4 | Drug Mixed with Two Polymers: Exposure to Water | 219 |
| 9.3.5 Drug Mixed with Biodegradable Polymer: Drug Elution | ||
| with Polymer Degradation | 220 | |
| 9.4 | Summary | 223 |
| References | 223 | |
| 10 | Raman Imaging of Plant Cell Walls | 225 |
| Notburga Gierlinger | ||
| 10.1 | Introduction | 225 |
| 10.2 | Plant Cell Walls | 226 |
| 10.3 | Micro-Raman Spectroscopy of Plant Fibers | 227 |
| 10.4 | Plant Cell Wall Imaging by Confocal Raman Microscopy | 228 |
| 10.4.1 Imaging Cellulose Orientation and Lignin Distribution | ||
| in Wooden Cell Walls | 228 | |
| 10.4.2 Silica and Cell Wall Composition in Horsetail | ||
| (E. hyemale) | 232 | |
| 10.5 | Outlook | 234 |
| 10.6 | Material and Methods | 234 |
| References | 235 | |
| 11 | Confocal Raman Imaging of Polymeric Materials | 237 |
| Ute Schmidt, Jörg Müller, and Joachim Koenen | ||
| 11.1 | Introduction | 237 |
| 11.2 | Raman Imaging of Isotactic Polypropylene (iPP) | 239 |
| 11.3 | Raman Imaging of Polymer Blends | 244 |
| 11.3.1 Raman Imaging of Thin Films of the Polymer Blend: | ||
| Polystyrene (PS)- Ethyl-Hexyl-Acrylate (EHA) | 245 | |
| 11.3.2 Raman Imaging of Thin Films of the Polymer | ||
| Blend Ethyl-Hexyl-Acrylate (EHA)-Styrene-Butadiene | ||
| Rubber (SBR) | 247 | |
| 11.3.3 Raman Imaging of Thin Films of the Polymer Blend | ||
| PS-EHA-SBR | 249 | |
| 11.4 | Polymer Coatings | 251 |
| 11.4.1 | Acrylic Paints | 251 |
| 11.4.2 | Adhesives | 253 |
| 11.5 | Additives in Polymer Matrices | 253 |
| 11.6 | Summary | 257 |
| References | 257 | |
| 12 | Stress Analysis by Means of Raman Microscopy | 259 |
| Thomas Wermelinger and Ralph Spolenak | ||
| 12.1 | Introduction | 259 |
| 12.1.1 | Theoretical B ackground | 260 |
| 12.1.2 Measuring in Conventional Back-Scattering | ||
| Configuration | 261 | |
| 12.1.3 | Off-Axis Raman Spectroscopy | 263 |
| 12.1.4 Stress Tensor Analysis in Back-Scattering | ||
| Raman Microscopy | 266 | |
| 12.2 | Case Studies | 268 |
| 12.2.1 | 3D Raman Spectroscopy Measurements | 268 |
| 12.2.2 | ZnO | 271 |
| 12.2.3 The Influence of Stress on the Peak Position | ||
| of Polymers | 273 | |
| 12.3 | Discussion | 276 |
| References | 277 | |
| Index | 279 | |
A
Abberation function, 5
Abbe, Ernst Karl, 2
Abiogenic MMC formation, 128
Accumulations, 71
Acquisition of spectra, 62
Acrylic latex, 252
Acrylics, 251
Active compound, 152
Active drug delivery systems, 139
Active pharmaceutical ingredients (API), 166
Active therapeutic coatings, 210
Adhesive, 191
Adhesive potential, 238
Aerogel, 118
Aerosol, 189
Ageing, 194
Agglomerative clustering, 79
Albumin, 146
Aliphatic compound, 115
Alkyd, 251,252
Alkyl chain length, 212
Alpha-PbC>2-structured TiÛ2, 125
Alteration history, 119
Alteration history of minerals, 112
Alteration veins, 113
American Food and Drug Administration
(FDA), 157, 196
Amorphous, 215
Amorphous carbon, 254
Amorphous silica, 225, 234
Amphiphilic molecules, 153
Ancient meteoritic materials, 124
Anisotropic units, 275
Antenna, 35
Antibodies, 138
Anti-oxidants, 254
Anti-Stokes scattering, 24
Antisymmetric stretch vibration, 25
Aperture angle, 6, 9, 10
API, 166
API particles, 184
Apoptosis, 158
Aqueous alteration products, 120
Asymmetric stretching C-C vibration, 274
Atomic Force Microscopy (AFM), 172, 237, 249
Atomic replacement, 124
Attenuated total reflectance (ATR) objectives, 175
Augmented classical least squares method
(aCLS), 212
Australasian tektite field, 125
Autofluorescence, 170
Average spectra, 84
B
Backbone bond, 275
Back gate voltage, 105
Background, 71
Background subtraction, 61, 70, 86
Background suppression, 46
Back scattered electrons (BSE), 171
Backscattering configuration, 261, 266
Bacteria differentiation, 33
Band structure, 102
Basal (0001) twinning system, 271, 272
Basis analysis, 57
Basis spectra, 82
Benzene ring modes, 246
Biaxially oriented polypropylene, 242
Biaxial stress, 263, 265
Binders, 251
Bioavailability, 178
Biocompatibility, 203
Biodegradable matrix, 185
polymer, 220
