Chemical Analysis and Material Characterization by Spectrophotometry

Description

Chemical Analysis and Material Characterization by Spectrophotometry integrates and presents the latest known information and examples from the most up-to-date literature on the use of this method for chemical analysis or materials characterization. Accessible to various levels of expertise, everyone from students, to practicing analytical and industrial chemists, the book covers both the fundamentals of spectrophotometry and instrumental procedures for quantitative analysis with spectrophotometric techniques. It contains a wealth of examples and focuses on the latest research, such as the investigation of optical properties of nanomaterials and thin solid films. Cover......Page 1 Chemical Analysis and Material Characterization by Spectrophotometry ......Page 2 2 - Theory and instrumentation of absorption spectroscopy: UV–VIS spectrophotometry and colorimetry......Page 3 6 - Introduction to nanomaterials and application of UV–Visible spectroscopy for their characterization......Page 4 1.2 Classification of spectroscopic techniques......Page 5 1.3.1 Fundamental properties of EM......Page 6 1.3.2.1 Absorption of light......Page 8 1.3.2.2 Transmission and reflection (visible light)......Page 11 1.3.2.3 Refraction of light......Page 14 1.3.2.5 Light scattering in media......Page 15 1.3.2.6 Diffraction of light......Page 16 1.3.2.7 Emission (fluorescence/phosphorescence)......Page 17 1.4.2 Numerical problems......Page 18 Further reading......Page 19 5.1 Types of chemical contamination in water/environment......Page 20 2.2.1 Absorption and emission processes (concept from quantum physics)......Page 21 2.2.3 Terms employed in absorption spectroscopy......Page 24 2.2.4 Beer-Lambert’s law: quantitative aspects of absorption measurements......Page 25 2.2.5 Application of Beer’s law......Page 27 2.2.6 Limitations to Beer’s law (deviation from Beer’s law)......Page 28 2.3.1.1 Continuous light source (continuum sources in the ultraviolet/visible region)......Page 30 2.3.2 Filter, monochromator and slit......Page 32 2.3.4 The detector......Page 33 2.3.4.2 Silicon photodiode......Page 34 2.4.3 Double-beam (DB)-in-time......Page 36 2.5.3 Resolution testing......Page 38 2.5.4.1 Problems......Page 39 Further reading......Page 41 C......Page 298 3.1.1 Why sample preparation is required?......Page 42 3.1.3 Classification of reagents and their choices for sample preparation......Page 43 3.1.4 Classification of acids......Page 44 3.1.5 Storage of samples and solutions......Page 47 3.1.6 Methods for weighing the samples and method for standard solution preparation......Page 48 3.1.6.1.4 Procedure for weighing samples......Page 49 3.1.6.1.5.2 Indirect weighing (weighing by difference)......Page 50 B......Page 51 Further reading......Page 53 4.1 Sampling......Page 54 4.2 Steps and important factors for sampling......Page 55 4.3.1 Systematic sampling......Page 57 5.2.2.1 Application of Beer's law......Page 89 6.3.1 Zero-dimensional (0-D) nanomaterials......Page 154 4.3.4 Stratified sampling......Page 58 4.4 Types of samples......Page 59 4.5 Sample size, preservations and analysis......Page 60 4.7 Dealing with sample matrix......Page 61 4.8 Dealing with variation in concentration range and sample stability......Page 62 4.9.1 Water sample......Page 63 4.9.2 Soil sampling, processing and storage......Page 66 4.9.3.1 Crushing of the rock sample......Page 68 5.2.1.2 Performance characteristics......Page 69 9.4.5 Lifetime measurements......Page 78 4.10.3 Results......Page 79 Further reading......Page 81 5 - Application of UV–VIS spectrophotometry for chemical analysis......Page 82 5.2.1.1 Basic terminology......Page 87 9.2.1 Electronic states of formaldehyde......Page 270 5.3 Instrument calibration (by External Standard Method)......Page 90 5.4.1.1.1 General discussion: Occurrence and effects......Page 91 5.4.1.1.5 Apparatus......Page 92 5.4.1.2.2 Principle......Page 93 5.4.1.2.6 Reagents......Page 95 5.4.1.2.10 Apparatus......Page 97 5.4.1.3.1 General discussion......Page 98 5.4.1.3.2 Sample storage......Page 99 5.4.1.3.5 Method......Page 100 5.4.1.4.1 Principle of the method......Page 101 5.4.1.4.4 Reagents......Page 102 5.4.1.5.1 General discussion......Page 103 5.4.1.5.5 Reagents......Page 104 5.4.1.5.7 Measurement procedure......Page 105 5.4.1.6.1 General discussion: forms of chlorine and effects of water chlorination......Page 106 5.4.1.6.2 Principle......Page 107 5.4.1.6.5 Apparatus......Page 108 5.4.1.7.1 Principle......Page 110 5.4.2.1.1 Discussion......Page 112 5.4.2.1.4 Apparatus and reagents......Page 113 5.4.2.2.4 Apparatus and reagents......Page 115 5.4.2.2.5 Procedure for sample preparation and measurements......Page 116 5.4.2.3.5 Apparatus and reagents......Page 117 5.4.2.3.6 Sample collection, preservation and storage......Page 118 5.4.2.3.7 Calibration, standardization and measurements......Page 119 5.4.2.4.2 Principle......Page 120 5.4.2.4.3.1 Persulphate method......Page 121 5.4.2.4.5 Apparatus and materials......Page 122 5.4.2.5.5 Apparatus and reagents......Page 124 5.4.2.6.1 Discussion......Page 125 5.4.4 Preparation of sample solutions of arsenate......Page 126 5.4.4.1 Measurement of the analyte solution......Page 127 5.4.5.1 Important terminologies used in interpretation of nature of absorption spectra......Page 128 5.4.5.2 Application of UV–Vis spectroscopy for qualitative information: understanding molecular structure from absorption spectra......Page 129 5.4.5.3.1.1 General discussion......Page 136 5.4.5.3.2.2 Reagents......Page 137 5.4.5.3.4.2 Principle......Page 138 5.4.5.3.5.1 General discussion......Page 139 5.4.5.3.6.1 General discussion......Page 140 5.4.5.3.6.2 Reagents......Page 141 5.4.5.3.8.2 Reagents......Page 142 5.4.5.3.9.2 Reagents......Page 144 5.4.5.3.10.1 Principle......Page 145 References......Page 147 6.1.1 Introduction......Page 149 6.1.2.1 Size and shape......Page 150 9.2.1.2 How do molecules release energy?......Page 153 6.3.2 One-dimensional nanomaterials......Page 155 6.3.4.1 Summary......Page 156 D......Page 157 6.5.2.1.1 Resistance heating evaporation......Page 158 6.5.2.1.3 Electrical arc discharge......Page 160 6.5.2.1.5 Sputtering......Page 161 6.5.2.1.5.2 Laser ablation (LA)......Page 163 6.5.2.2 Chemical methods......Page 164 6.5.2.2.1 APCVD (atmospheric pressure CVD)......Page 166 6.5.2.2.3.1 CVD sources and substrates......Page 167 6.5.2.2.4.1 Pyrolytic LCVD......Page 168 6.5.2.2.5 Atomic layer deposition (ALD)......Page 169 6.5.2.2.6.1 (I) Spray pyrolysis......Page 170 6.5.2.2.6.2 Spin coating......Page 172 6.5.2.2.6.3 Hydrothermal......Page 173 6.5.2.2.6.5 Electro-deposition......Page 175 6.5.2.2.6.6 Electroless deposition......Page 176 6.6.1 Material properties......Page 177 6.6.2 Analytical techniques (overview)......Page 179 6.6.3.1 Particle size and dispersions......Page 181 6.6.3.4 Composition......Page 182 6.6.3.6 Optical properties (of nanomaterials based thin films)......Page 183 6.6.5.1 Transmittance (T) of semiconductor thin films......Page 188 6.7 Questions......Page 198 Further reading......Page 199 7.2 IR radiation and relatio with molecular properties......Page 201 7.3 EM and molecular excitations......Page 202 7.3.3 Relation between energy change (due to transition) and frequency of radiation frequency......Page 203 7.5.1 Number of vibrational frequencies and IR spectra......Page 205 7.5.3 Types of vibrations......Page 206 7.5.4 Models for understanding the molecular vibration......Page 207 7.6 Selection rules for infrared transitions......Page 210 7.6.1 Concept from quantum theory......Page 211 7.6.2 Overtones......Page 212 7.8.1 Coupling interactions due to stretching vibrations......Page 213 8.7.3.6 Solid samples......Page 263 7.8.2 Coupling interactions due to bending vibrations......Page 214 7.8.4 Coupling due to interactions between fundamental vibrations and overtones (fermi resonance)......Page 215 7.10 Instrument designs for infrared absorption......Page 217 7.10.1 Sample illumination system (light source)......Page 218 7.10.2 Monochromators......Page 219 7.10.3 Sample holding system (sample cells)......Page 220 7.11.1 Filter photometers......Page 222 7.11.2 Double-beam spectrophotometer......Page 223 7.11.4 Attenuated total reflectance (ATR) FT–IR instrument......Page 224 7.12 Applications of IR spectroscopy......Page 226 7.12.1 Interpretation of IR spectra......Page 227 7.12.2 Qualitative application: spectral searching method (for identifying unknown or new compound)......Page 234 7.12.4 Application of FTIR in material characterization......Page 235 7.12.4.1 Highlights of properties of some promising materials and their applications: graphene based materials (GBMs)......Page 237 8.7.3.4 Gas samples......Page 238 7.12.4.3 Overview of unique properties and applications of methylammonium leadhalide (MALH) perovskite in thin film based solar cells......Page 239 Further reading......Page 244 8.1 Introduction......Page 246 8.3.1 Basic concept of molecular polarizability (polarizability under static electric field)......Page 248 8.3.2 Sources of polarizability......Page 250 8.3.3 Polarizability due to the interaction of light with a molecule......Page 251 8.3.4 Classical (wave) model of Raman and Rayleigh scattering......Page 252 8.4 Selection rule......Page 255 8.5 Comparison/contrast between IR spectroscopy and Raman spectroscopy......Page 257 8.7 Experimental setup......Page 260 8.7.2 Filters/grating......Page 261 8.7.3 Detectors (transducer)......Page 262 8.8.1 Raman spectra of inorganic species......Page 264 8.8.2 Raman spectra of organic species......Page 265 8.9 Application of Raman spectroscopy in material science......Page 266 Further reading......Page 268 9.2.1.1 What happens after absorption of light energy?......Page 271 9.3.1.1 Vibrational relaxation, vr......Page 274 9.3.2.1 Fluorescence emission......Page 275 9.3.2.2 Quantitative relation between analyte concentration and fluorescence......Page 276 9.3.2.3 Phosphorescence emission......Page 278 9.3.3 Chemiluminescence (excitation by chemical process and relaxation by photon emission)......Page 279 9.4.1 Brief overview of components for fluorescence measurements......Page 280 9.4.3 Excitation versus emission spectra......Page 281 9.4.4 Relationship between absorption and emission spectra......Page 282 9.4.5.2 Methods to determine fluorescence lifetime of fluorophores......Page 284 9.5 Instrument standardization method......Page 285 9.6.1 Analyte's Concentration determination......Page 286 9.6.1.1 Determination of quinine in urine......Page 288 9.6.2.1 GO and rGO......Page 291 9.6.3.3 Fluorescence lifetime imaging (FLI)......Page 292 9.7 Questions......Page 293 References......Page 295 G......Page 299 M......Page 300 R......Page 301 S......Page 302 Z......Page 303 Back Cover......Page 304